CN105158551B - A kind of method of single ion signal in measurement flight time mass spectrum - Google Patents
A kind of method of single ion signal in measurement flight time mass spectrum Download PDFInfo
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- CN105158551B CN105158551B CN201510492655.XA CN201510492655A CN105158551B CN 105158551 B CN105158551 B CN 105158551B CN 201510492655 A CN201510492655 A CN 201510492655A CN 105158551 B CN105158551 B CN 105158551B
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Abstract
The present invention relates to ionization time of flight, specially a kind of method for measuring single ion signal in flight time mass spectrum.Solve the technical problem for being difficult to the single ionic strength of accurately detecting in current ionization time of flight.The present invention makes ion gun to be measured launch ion with impulse form by conventional technical means, and then detects reception by ion detector, and the signal peak of ion is finally obtained on digital oscilloscope；The triggering level of digital oscilloscope is adjusted, the signal intensity of ion gun launch ion in a pulse can be obtained under each triggering level, that is, obtains the relation of a triggering level and the ion signal intensity of an impulse ejection；The ion signal intensity level under multiple triggering levels is recorded, corresponding image is drawn, the signal intensity of single ion counter can be just released by linear fit.This method is simple to operate, and measurement result accuracy is high.
Description
Technical field
It is specially a kind of to measure single ion signal in flight time mass spectrum the present invention relates to ionization time of flight
Method.
Background technology
The general principle of flight time mass spectrum is after charged ion obtains certain kinetic energy under accelerating field effect, quickly to fly
Row is to detector so as to detected.Generally for the voltage signal for obtaining observable, can also electron multiplication and electricity be carried out to signal
Press big processing.Because the charge-mass ratio of charged ion can influence the time of ion arrival detector, therefore flight time mass spectrum
It is an important identification technology in current mass spectrometer.Flight time mass spectrum has that time response is fast, spatial resolution is strong
And detectivity it is high the features such as, be widely used in the high-tech areas such as all kinds of basic scientific researches, Aero-Space, with
The technical fields such as the closely bound up food security of the people's livelihood, biological medicine, environmental monitoring, also there is quite varied purposes.
Ion signal on flight time mass spectrum is in impulse type pointed shape.The time that voltage signal occurs depends on ion
Charge-mass ratio, the flying distance of accelerating potential and ion.Number, energy and the spatial distribution of ion signal can influence from
The intensity amplitude and time width of subsignal.Therefore people generally select the area of voltage signal, i.e., voltage strength is to the time
Integration, to characterize the intensity of ion signal, the relatively strong and weak of ion signal is characterized with the relative size of area figures.Flight time
Mass spectrographic hypersensitivity allows it to detect a small number of ions, it might even be possible to detect single ion.Therefore single ion is obtained
The specific strength values of signal are most important to quantitative analysis time mass spectrum.But shortage is a kind of easily operated at present and being capable of essence
Really know the method for single ion signal intensity.
The content of the invention
The present invention is the technical problem for solving to be difficult in current ionization time of flight the single ionic strength of accurately detecting,
A kind of method for measuring single ion signal in flight time mass spectrum is provided, one kind is provided for quantitative analysis time mass spectrum and is easy to
Operation, practicable general technology.
The present invention is realized using following technical scheme：The side of single ion signal in a kind of measurement flight time mass spectrum
Method, comprises the following steps：
（a）Ion gun to be measured is controlled to launch ion with impulse form；The ion launched by ion gun to be measured is in accelerating field
In the presence of accelerate to fly to after ion detector and be converted into corresponding current signal in vacuum environment, be reconverted into corresponding
Voltage signal, and be amplified, digital oscilloscope is recently entered, obtains being rendered as the ion signal of signal peak；
（b）The triggering level of digital oscilloscope is adjusted, for each triggering level, a phase is obtained using Lorentz fit
The area value that induction signal peak is surrounded, that is, the ion signal of an impulse ejection intensity, and then obtain different triggering levels
The intensity of the ion signal of next pulse transmitting；
（c）Data according to being obtained in previous step draw the intensity of ion signal and the relation curve of triggering level, and
Linear fit is carried out, according to the anti-peak area for releasing ion signal when triggering level is zero of fitting result, that is, single ion is obtained
The intensity level of signal.
The present invention makes ion gun to be measured launch ion with impulse form by conventional technical means, and then passes through ion detection
Device detection is received, and the signal peak of ion is finally obtained on digital oscilloscope；The triggering level of digital oscilloscope is adjusted, each
The signal intensity of ion gun launched ion in a pulse can be obtained under triggering level, that is, obtains a triggering electricity
The flat relation with the ion signal intensity of an impulse ejection；The ion signal intensity level under multiple triggering levels is recorded, is drawn
Corresponding image, the signal intensity of single ion counter can be just released by linear fit.
The method of the invention is applicable to different ion guns to be measured, only ion gun to be measured need to be controlled to be sent out with impulse form
Penetrate ion.Described ion detector, accelerating field etc. is the ordinary skill in the art.Lorentz fit can be improved
To the computational accuracy of signal peak area value.
Further, step（b）In ion source signal is repeatedly measured under each triggering level, that is, obtain each triggering
The ion signal of multiple pulses under level, then averages again, as an impulse ejection under the triggering level from
The intensity of subsignal.
Averaging can make final result more accurate reliable.
Further, step（a）Middle control ion gun launches ion with nanosecond pulse.
Nanosecond pulse ensure that the amount of ions of each impulse ejection is few, and can ensure ion on time mass spectrum
The time resolution of signal, thus can further improve the accuracy of measurement.
The present invention uses Lorentz fit and linear fit, and then the anti-signal intensity for releasing single ion, side used
Method result is accurately reliable, operates very simple, can apply to the detection to different kinds of ions source.
Brief description of the drawings
The schematic device of single ion signal in Fig. 1 measurement flight time mass spectrums.
1- vacuum chambers；2- ionic pumps；3- ion guns to be measured；4- accelerates aperture plate；5- microchannel plates；6- stainless steel electrodes；7-
Accelerate aperture plate power supply；8- microchannel plate power supplies；9- digital delay impulse generators；10- ion source controllers；11-
Digital oscilloscope；12- pulse signal amplifiers；13- triggering level controllers.
Fig. 2 flight time mass spectrums.Triggering level in figure is 8mV, and solid black lines are that data A is in Lorentz fit, figure
The area of peak-to-peak signal.
The relation of Fig. 3 ion signals integral area and triggering level.Linear fit obtains the area with y-axis intersection point in figure
Value 0.27V (4) * ns, i.e., corresponding to single Cs atom ion signal intensity.
Embodiment
The structural representation of equipment therefor when Fig. 1 is concrete application of the present invention.
Sign 1 is a vacuum chamber, and pressure reaches 10-3-10-4Pa.In this experiment, vacuum pressure can reach
10-7Pa, vacuum is maintained by ionic pump.It is the most basic structure of flight time mass spectrum in vacuum cavity：Sign 4 is an acceleration
Aperture plate, constant voltage is provided by acceleration aperture plate power supply 7；Sign 3 is ion gun to be measured, and this experiment uses alkali metal former
The ion gun of sub- caesium.Sign 5 is two pieces of microchannel plates, is separated with the circular ring plate of thin stainless steel therebetween.In order to reduce detection
The noise of signal, the channel direction of microchannel plate is oppositely positioned.Sign 8 is the power supply of microchannel plate.Sign 6 be one piece not
Become rusty steel electrode（Collector）.Sign 9 is a digital delayed-pulse generator, can produce the nanosecond order even arteries and veins of picosecond magnitude
Rush control signal.Sign 10 is an ion source controller, the generation for controlling ion gun.Sign 10 is specifically adopted in this experiment
With a pulsed dye laser, the light pulse that width is 8ns can be produced.Sign 12 is pulse signal amplifier, and its function is
The current signal of stainless steel electrode is converted into voltage signal, and is amplified.Sign 11 is a digital oscilloscope.For remembering
Record and the signal of storage flight time mass spectrum.Sign 13 is the triggering level controller of digital oscilloscope.
During specific detection, the control signal that digital delay impulse generator 9 produces nanosecond order is input to ion gun control
Device 10, produces the light of nanosecond pulse, and then obtains the ion gun of nanosecond pulse（Sign 3）.Or by making acceleration aperture plate power
Power supply 7 produces nanosecond pulse voltage, can equally obtain the ion gun of nanosecond pulse.Ion gun is accelerating adding for the generation of aperture plate 4
Accelerate to fly to ion detector in the presence of fast electric field（It is made up of sign 5,6,8）, by electron multiplication effect obtain it is a large amount of
Electronically form electric current.Voltage signal is converted electrical current into by pulse signal amplifier 12, and is amplified, numeral is finally passed through
Oscillograph 11.
The first step：The triggering level of triggering level controller 13 is adjusted, different triggerings can be recorded on digital oscilloscope
Ion signal under level, the integral area of current versus time is obtained through data processing.When Fig. 2 is that triggering level is set to 8mV,
The flight time mass spectrum signal for the typical Cs atom ion of a width that digital oscilloscope is collected.The depression of signal is deeper, width
The bigger electron number represented after electron multiplication is more.Due to there is the electronics such as electric capacity in collection signal circuit and amplification potential circuit
Element so that voltage signal vibrates.The area value of peak-to-peak signal can be obtained using Lorentz fit, you can obtain ion letter
Number intensity.
Second step：Measure a series of flight time mass spectrum of the Cs atom ion under triggering levels.In identical triggering level
Lower repeatedly measurement, averages, draws the integral area of ion signal（The area value obtained after Lorentz fit）With touching
Generate electricity flat relation, carries out the area figures that linear fit obtains characterizing the intensity of single ion signal.Fig. 3 is the knot of test
Really.It can be seen that with the increase of triggering level, the area of ion signal is linearly increased.Linear fit is carried out, it is counter to shift triggering electricity onto
Put down the quantificational expression that area when being zero is single ionic strength.
Explanation：1. when carrying out single ion ionization meter using the method for the invention, the number of ion gun should be caused to use up
Amount is few.2. carry out single ion ionization meter using the method for the invention on other devices, the change of partial devices, example
Such as ion gun, ion detector, when amplifier etc. changes, the single ion area of acquisition is also different.But described device, especially
Method has versatility.Obtaining single ion signal intensity just can carry out quantitative analysis.
Claims (2)
1. a kind of method for measuring single ion signal in flight time mass spectrum, it is characterised in that comprise the following steps：
（a）Ion gun to be measured is controlled to launch ion with impulse form；Work of the ion launched by ion gun to be measured in accelerating field
Acceleration is flown to after ion detector and is converted into corresponding current signal in vacuum environment under, is reconverted into corresponding voltage
Signal, and be amplified, digital oscilloscope is recently entered, obtains being rendered as the ion signal of signal peak；
（b）The triggering level of digital oscilloscope is adjusted, for each triggering level, a corresponding letter is obtained using Lorentz fit
The area value that number peak is surrounded, that is, the ion signal of an impulse ejection intensity, and then it is next to obtain different triggering levels
The intensity of the ion signal of individual impulse ejection；In this step, ion source signal is repeatedly measured under each triggering level, that is, obtained
The ion signal of multiple pulses under each triggering level is obtained, then averages again, is used as an arteries and veins under the triggering level
Rush the intensity of the ion signal of transmitting；
（c）Data according to being obtained in previous step draw the intensity of ion signal and the relation curve of triggering level, and carry out
Linear fit, according to the anti-peak area for releasing ion signal when triggering level is zero of fitting result, that is, obtains single ion signal
Intensity level.
2. a kind of method for measuring single ion signal in flight time mass spectrum as claimed in claim 1, it is characterised in that step
Suddenly（a）Middle control ion gun launches ion with nanosecond pulse.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689134A (en) * | 2002-07-16 | 2005-10-26 | 力可公司 | Tandem time of flight mass spectrometer and method of use |
| CN102884608A (en) * | 2010-01-15 | 2013-01-16 | 莱克公司 | Ion trap mass spectrometer |
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| GB2445169B (en) * | 2006-12-29 | 2012-03-14 | Thermo Fisher Scient Bremen | Parallel mass analysis |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1689134A (en) * | 2002-07-16 | 2005-10-26 | 力可公司 | Tandem time of flight mass spectrometer and method of use |
| CN102884608A (en) * | 2010-01-15 | 2013-01-16 | 莱克公司 | Ion trap mass spectrometer |
Non-Patent Citations (3)
| Title |
|---|
| 单颗粒气溶胶飞行时间质谱仪在细颗粒物研究中的应用和进展;蔡靖 等;《分析化学》;20150531;第43卷(第5期);第1-5节 * |
| 飞行时间质谱中的空间电荷效应研究;石勇;《物理化学学报》;20051231;第21卷(第11期);第1269-1273页 * |
| 飞行时间质谱探测磁光阱中超冷分子离子的实验研究;元晋鹏 等;《物理学报》;20121231;第61卷(第18期);第183301-1至183301-6页 * |
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