CN108169320A - The laser mass spectrometry measuring method of one trace elements and normal pressure open type Portable laser mass spectrograph - Google Patents
The laser mass spectrometry measuring method of one trace elements and normal pressure open type Portable laser mass spectrograph Download PDFInfo
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- 238000000322 laser mass spectrometry Methods 0.000 title claims abstract description 15
- 230000005284 excitation Effects 0.000 claims abstract description 25
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—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
- G01N27/64—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 wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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Abstract
The present invention provides the laser mass spectrometry measuring method of a trace elements and normal pressure open type Portable laser mass spectrographs, belong to field of analytic instrument.When this programme is measured for trace element using mass spectrograph, since its content is extremely low, lead to detection difficult and relatively low signal-to-noise ratio, resonant excitation is carried out so as to select the laser of corresponding wavelength according to the jump frequency of object element atom, lewis' acid, the ionization rate of element to be measured is selectively improved, therefore can accomplish selectively to detect object, improves the signal-to-noise ratio of object to be detected, the concentrations of object to be detected are reduced, are suitable for tailored version detection.
Description
Technical field
The present invention relates to field of analytic instrument, the laser mass spectrometry measuring method and normal pressure for referring in particular to a trace elements open
Open type Portable laser mass spectrograph.
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
With chemical composition present in the abundance of gaseous ion identification sample containing amount and type, 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, secondly 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 the mass spectroscopy device of nearly 500,000,000 dollars 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 it is portable
Formula open air in-situ measuring method and relevant device become the recent focus of attention.Regrettably traditional mass spectrograph is all true
Sky is lower to be operated, and 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),
It the methods of Matrix Assisted Laser Desorption ionization (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)
Wait the invention of 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. auxiliary device is needed to crush sample, dissolves even atomization process.
Current antivacuum mass-spectrometer measurement there are the defects of both be from the deficiency of ionization method itself.Either ESI is also
The methods of being DART, use is all electronics or ion injection method charge sample.Such soft ionization method is to easy
Desorption, volatile, soluble material is very applicable, but for hard, non-volatile, indissoluble, infusibility, the difficult sample ionized just
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.
The defects of for above-mentioned vacuum mass spectrometer, is substituted using normal pressure open type Portable laser mass spectrograph.This sets
Standby to use a laser as ion source, 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, without any additional system
Sample, sampling and sample introduction facility can realize that the normal pressure open type of real meaning exempts from sample preparation measurement.By being acquired in the method
Be the plasma generated after laser bombardment, therefore ionic species contained in plasma (has in laser irradiation process
Imitate the sample molecule or atom of ionization) determine ingredient in the sample that can effectively detect.For micro and trace
Element detection (such as ppb grades even Element detection of Asia ppb concentration), since contained amount is extremely low, leads to detection difficult and relatively low
Signal-to-noise ratio.
Invention content
The technical problems to be solved by the invention are：Normal pressure open type Portable laser mass spectrograph measures trace element in sample
When, since constituent content to be surveyed is extremely low, lead to detection difficult and relatively low signal-to-noise ratio.
In order to solve the above-mentioned technical problem, the invention discloses the laser mass spectrometry measuring method of a trace elements, the party
Method specifically may include following steps：
S1, the resonant frequency for determining trace element to be surveyed in sample to be tested；
S2, the laser that specific wavelength corresponding with the frequency is selected according to the resonant frequency of gained；
S3, using the laser of selected specific wavelength carry out irradiation survey and resonant excitation trace element to be surveyed, the resonance swash
Hair process is Single-photon ionization or multiphoton ionization；
S4, the trace element to be surveyed of resonant excitation is measured using the mass analyzer of laser mass spectrometry instrument.
On the basis of said program, in the S3 steps, the laser of the specific wavelength directly irradiates bombardment sample to be tested
And resonant excitation element to be surveyed.
On the basis of said program, in the S3 steps, plasma to be measured is formed first with a laser bombardment sample to be tested
Then body recycles the laser of the specific wavelength to irradiate plasma to be measured and resonant excitation element to be measured.
In addition, with reference to the above method, this programme also discloses a kind of normal pressure open type Portable laser mass spectrograph, specific to wrap
It includes：Control unit, the first laser device being connected with control unit, the mass analyzer being connected with control unit, further including can be right
Generated laser beam carries out the first light path system of shaping, transmission, direction and focusing in the laser, and for shape
Normal pressure open type into sample to be tested plasma ionizes chamber, and the first light path system can be by laser produced by first laser device
In guiding to ionization chamber；
The first laser device is that can form the laser of specific wavelength corresponding with element resonant frequency to be surveyed.
Further, the first laser device is tunable laser.
Further, it is certain long wavelength laser that the first laser device, which is selected, which resonates according to element to be surveyed
Frequency is determined.
Further, produced laser can be directed to ionization chamber through the first light path system in the first laser device
In sample on.
In addition, normal pressure open type Portable laser mass spectrograph further includes to bombard sample to be tested and generate the of plasma
Dual-laser device and the second light path system corresponding with second laser, the second light path system can will be produced by second lasers
Laser aiming to the ionization chamber, second laser is also connected with described control unit.
Further, produced laser can be directed to ionization chamber through the second light path system in the second laser
In sample to be tested on and bombard sample to be tested and form plasma, produced laser can be through the first light in the first laser device
Road system is directed on the plasma formed in ionization chamber simultaneously resonant excitation plasma.
Further, the normal pressure open type Portable laser mass spectrograph further includes laser beam obstruction device, is worn for stopping
Cross the plasma to be measured non-irradiated laser beam on sample to be tested.
When this programme is measured for trace element using mass spectrograph, since its content is extremely low, cause detection difficult and
Relatively low signal-to-noise ratio, so as to which the laser of resonant wavelength laser can be provided using the method and correspondence of laser resonant excitation, from
And optionally resonant excitation element to be surveyed, therefore optionally detect object, the signal-to-noise ratio of object to be detected is improved, is dropped
The concentrations of low object to be detected are suitable for tailored version detection.
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 structure diagram of normal pressure open type Portable laser of the present invention；
Fig. 2 is the mass spectrometric structure diagram of another normal pressure open type Portable laser of the present invention.
In figure, 1- mass analyzers, 2- control units, 3- first laser devices, the first light path systems of 4-, 5- plasmas,
6- samples, 7- second lasers, the second light path systems of 8-, 9- laser beam obstruction devices.
Specific embodiment
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, the laser mass spectrometry measuring method of a trace elements is disclosed, this method can specifically wrap
Include following steps：
S1, the resonant frequency for determining trace element to be surveyed in sample to be tested；
S2, the laser that specific wavelength corresponding with the frequency is selected according to the resonant frequency of gained；
S3, using the laser of selected specific wavelength carry out irradiation survey and resonant excitation trace element to be surveyed, the resonance swash
Hair process is Single-photon ionization or multiphoton ionization, and multiple photons can be identical energy or different-energy, can
Transition is realized by absorbing the energy of photon；
S4, the trace element to be surveyed of resonant excitation is measured using the mass analyzer of laser mass spectrometry instrument.This programme
In, key ideas be using with element resonant frequency to be surveyed corresponding to wavelength laser come selectively resonant excitation sample
In element to be measured, improve the signal-to-noise ratio of object to be detected, reduce the concentrations of object to be detected, be suitable for tailored version detection.
On the one hand can be that the laser of the specific wavelength directly irradiates in the S3 steps on the basis of said program
Bombard sample to be tested and resonant excitation element to be surveyed.On the other hand it is or (non-with resonating in survey element first with a laser
The laser of frequency corresponding wavelength) bombardment sample to be tested form plasma to be measured, then recycle the laser of the specific wavelength
Irradiate plasma to be measured and resonant excitation element to be measured.
With reference to Fig. 1, in one embodiment, with reference to the above method, this programme also discloses a kind of normal pressure open type just
Laser mass spectrometry instrument is taken, is specifically included：Control unit 2, the first laser device 3 being connected with control unit 2 are connected with control unit 2
Mass analyzer 1, shaping, transmission, direction and focusing can be carried out to generated laser beam in the laser by further including
The first light path system 4 and be used to form sample to be tested plasma 5 normal pressure open type ionization chamber, the first light path
System 4 can extremely ionize laser aiming produced by first laser device 3 in chamber；
The first laser device 3 is that can form the laser of specific wavelength corresponding with element resonant frequency to be surveyed, described
Produced laser can be directed to through the first light path system 4 on the sample 6 in ionization chamber in one laser 3.In the program
Laser mass spectrometry instrument, used first laser device 3 can generate and the laser of element resonant frequency corresponding wavelength to be surveyed,
Its specific type can be preferably tunable laser or the first laser device 3 also can be selected as certain long wavelength laser,
The standing wave length is determined according to element resonant frequency to be surveyed.Either that laser, purport are all to generate and be intended to
Survey the laser of element resonant frequency corresponding wavelength.Element to be surveyed in sample to be tested 6 adjusts the wavelength of first laser device 3
Either select the laser of specific wavelength so that it sends out the laser of specific wavelength to first laser, and in the first light path system 4
Under the action of, the laser of specific wavelength is directed among ionization chamber, under the irradiation of specific wavelength laser, on the one hand may be used
It bombards sample 6 and generates plasma 5, while the laser of the specific wavelength of the first laser device 3 also can resonant excitation element to be surveyed
Then the either atom in molecule, molecule or group etc. are measured again via mass analyzer 1, are analyzed, accomplish may be selected
Property resonant excitation element to be surveyed, therefore optionally detect object, improve the signal-to-noise ratio of object to be detected, reduce to be detected
The concentrations of object are suitable for tailored version detection.
In addition, with reference to Fig. 2, in another embodiment, normal pressure open type Portable laser mass spectrograph further includes to be treated for bombarding
Sample 6 and generate plasma 5 second laser 7 and with 7 corresponding second light path system 8 of second laser, second
Light path system 8 can by laser aiming produced by second laser 7 to the ionization chamber, second laser 7 also with the control
Unit 2 processed is connected.Produced laser can be directed to through the second light path system 8 in ionization chamber in the second laser 7
Sample to be tested 6 on and bombard sample to be tested 6 and form plasma 5, produced laser can be through first in the first laser device 3
Light path system 4 is directed on the plasma 5 formed in ionization chamber simultaneously resonant excitation plasma 5.That is this reality
The laser mass spectrometry instrument applied in a scheme includes two lasers, wherein, second laser 7 is used to generate laser and in the second light path
System 8 is directed to ionization chamber and bombards sample to be tested 6 and form plasma 5 under acting on, which includes being intended to
The element of measurement and other a variety of non-it need to measure element etc..At the same time, first laser device 3 is recycled to be formed and element to be surveyed
The laser of resonant frequency corresponding wavelength, the laser of the specific wavelength to ionization chamber and resonate through the conduction of the first light path system 4
The formed plasma 5 of excitation, then measures again via mass analyzer 1, analyzes, accomplish optionally to resonate sharp
Hair element to be surveyed, therefore optionally detect object, the signal-to-noise ratio of object to be detected is improved, the detection for reducing object to be detected is dense
Degree is suitable for tailored version detection.
In addition, the normal pressure open type Portable laser mass spectrograph further includes laser beam obstruction device 9, the laser beam is utilized
Obstruction device 9 can be stopped across the plasma 5 to be measured non-irradiated laser beam on sample to be tested 6.
This programme is directed in the prior art, when trace element is measured using normal pressure open type Portable laser mass spectrograph,
Due to element to be surveyed, content itself is extremely low, so as to cause the technical problems such as detection difficult and relatively low signal-to-noise ratio, this hair of one side
It is bright to specifically disclose a kind of using laser resonant excitation element to be surveyed, the method then measured again.On the other hand utilizing should
Method corresponding laser that resonant frequency corresponding wavelength laser can be provided using one in normal pressure open-type laser mass spectrograph, utilizes
The laser then optionally resonant excitation element to be surveyed, therefore optionally detect object, improve the letter of object to be detected
It makes an uproar and compares, reduce the concentrations of object to be detected, be suitable for tailored version detection.
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 directly or indirectly used in other related technical areas, is similarly included in
In the scope of patent protection of the present invention.
Claims (10)
1. the laser mass spectrometry measuring method of a trace elements, which is characterized in that include the following steps：
S1, the resonant frequency for determining trace element atom to be surveyed in sample to be tested, ion or molecule；
S2, the laser that specific wavelength corresponding with the frequency is selected according to the resonant frequency of gained；
S3, irradiation survey and resonant excitation trace element to be surveyed, the resonant excitation mistake are carried out using the laser of selected specific wavelength
Journey is Single-photon ionization or multiphoton ionization；
S4, the trace element to be surveyed of resonant excitation is measured using the mass analyzer of laser mass spectrometry instrument.
2. the laser mass spectrometry measuring method of a trace elements as described in claim 1, which is characterized in that the S3 steps
In, the laser of the specific wavelength directly irradiates bombardment sample to be tested and resonant excitation element to be surveyed.
3. the laser mass spectrometry measuring method of a trace elements as described in claim 1, which is characterized in that the S3 steps
In, plasma to be measured is formed first with a laser bombardment sample to be tested, the laser of the specific wavelength is then recycled to irradiate
Plasma to be measured and resonant excitation element to be measured.
4. a kind of normal pressure open type Portable laser mass spectrograph using method as described in claim 1, which is characterized in that including：
Control unit, the first laser device being connected with control unit, the mass analyzer being connected with control unit, further including can be to described
Generated laser beam carries out the first light path system of shaping, transmission, direction and focusing in laser, and is used to form and treats
The normal pressure open type ionization chamber of sample plasma, the first light path system can be by laser aiming produced by first laser device
Into ionization chamber；
The first laser device is that can form the laser of specific wavelength corresponding with element resonant frequency to be surveyed.
5. normal pressure open type Portable laser mass spectrograph as claimed in claim 4, which is characterized in that the first laser device is can
Tuned laser.
6. normal pressure open type Portable laser mass spectrograph as claimed in claim 4, which is characterized in that the first laser device is selected
For certain long wavelength laser, which is determined according to element resonant frequency to be surveyed.
7. such as claim 4-6 any one of them normal pressure open type Portable laser mass spectrographs, which is characterized in that described first swashs
Produced laser can be directed to through the first light path system on the sample in ionization chamber in light device.
8. such as claim 4-6 any one of them normal pressure open type Portable laser mass spectrographs, which is characterized in that further include and be used for
Bombardment sample to be tested simultaneously generates the second laser of plasma and the second light path system corresponding with second laser, the
Two light path systems can by laser aiming produced by second laser to the ionization chamber, second laser also with the control
Unit is connected.
9. normal pressure open type Portable laser mass spectrograph as claimed in claim 8, which is characterized in that institute in the second laser
It generates on the sample to be tested that laser can be directed to through the second light path system in ionization chamber and bombards sample to be tested formation etc.
Gas ions, produced laser can be directed to through the first light path system formed in ionization chamber in the first laser device
On plasma and the resonant excitation plasma.
10. normal pressure open type Portable laser mass spectrograph as claimed in claim 9, which is characterized in that the normal pressure open type is just
It takes laser mass spectrometry instrument and further includes laser beam obstruction device, it is non-irradiated to sample to be tested across plasma to be measured for stopping
Laser beam.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112394119A (en) * | 2020-11-26 | 2021-02-23 | 长春理工大学光电信息学院 | Detection method for determining organochlorine pesticide components by gas chromatography-mass spectrometry |
| CN115295392A (en) * | 2022-07-11 | 2022-11-04 | 中国科学院上海技术物理研究所 | Laser secondary selective ionization isotope mass spectrometry method |
| CN115389602A (en) * | 2022-04-10 | 2022-11-25 | 宁波华仪宁创智能科技有限公司 | Security inspection device and method with trace detection function |
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