CN105158551A - Method for measuring single ion signal in time of flight mass spectrometry - Google Patents
Method for measuring single ion signal in time of flight mass spectrometry Download PDFInfo
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- CN105158551A CN105158551A CN201510492655.XA CN201510492655A CN105158551A CN 105158551 A CN105158551 A CN 105158551A CN 201510492655 A CN201510492655 A CN 201510492655A CN 105158551 A CN105158551 A CN 105158551A
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Abstract
The invention relates to the technology of time of flight mass spectrometry and particularly relates to a method for measuring a single ion signal in time of flight mass spectrometry, and solves the technical problem that the single ion intensity is hard to be precisely detected by the current technology of time of flight mass spectrometry. According to the invention, a to-be-tested ion source is enabled to emit ions in a pulse manner through a conventional technical means, ions are detected and received through an ion detector further, and an ion signal peak is obtained on a digital oscilloscope. Trigger levels of the digital oscilloscope are adjusted, the signal intensity of ions emitted by the ion source in a pulse under each trigger level is obtained, that is to say, the relation between one trigger level and the signal intensity of ions emitted by one pulse is obtained. Ion signal intensity values under multiple trigger levels are recorded, corresponding images are drawn, and the single ion signal intensity can be reversely derived through linear fitting. The method is simple to operate and the measurement result is high in accuracy.
Description
Technical field
The present invention relates to ionization time of flight, be specially a kind of method measuring single ion signal in flight time mass spectrum.
Background technology
The ultimate principle of flight time mass spectrum is after charged ion obtains certain kinetic energy under accelerating field effect, and rapid flight is to detector thus be detected.Generally for and obtain observable voltage signal, also can carry out the process of electron multiplication and voltage amplification to signal.Specific charge due to charged ion can affect the time that ion arrives detector, and therefore flight time mass spectrum is an important recognition technology in current mass spectrometer.Flight time mass spectrum has the strong and detection sensitivity high of fast, spatial resolution time response, be widely used in the high-tech areas such as all kinds of basic scientific research, Aero-Space, in technical fields such as the food security closely bound up with the people's livelihood, biological medicine, environmental monitorings, also there is purposes very widely.
Ion signal on flight time mass spectrum is impulse type pointed shape.The time that voltage signal occurs depends on the flying distance of the specific charge of ion, accelerating potential and ion.The number of ion signal, energy and space distribution all can affect intensity amplitude and the time width of ion signal.Therefore people select the area of voltage signal usually, and namely voltage strength is to the integration of time, characterize the intensity of ion signal, characterize the relatively strong and weak of ion signal by the relative size of area figures.The hypersensitivity of flight time mass spectrum makes it can detect minority ion, even can detect single ion.Therefore the concrete strength values obtaining single ion signal is most important to quantitative test time mass spectrum.But lack at present and be a kind ofly easy to operate and accurately can know the method for single ion signal intensity.
Summary of the invention
The present invention solves the technical matters being difficult to the single ionic strength of accurately detecting in current ionization time of flight, a kind of method measuring single ion signal in flight time mass spectrum is provided, operation is easy to, practicable current techique for quantitative test time mass spectrum provides one.
The present invention realizes by the following technical solutions: a kind of method measuring single ion signal in flight time mass spectrum, comprises the steps:
A () controls ion gun to be measured with impulse form emitting ions; The ion launched by ion gun to be measured is converted into corresponding current signal accelerate to fly to ion detector in vacuum environment under the effect of accelerating field after, be converted to corresponding voltage signal again, and amplify, finally input digital oscilloscope, obtain the ion signal being rendered as signal peak;
B () regulates the triggering level of digital oscilloscope, for each triggering level, Lorentz fit is utilized to obtain the area value of a corresponding signal peak encirclement, the namely intensity of the ion signal of an impulse ejection, and then the intensity obtaining the ion signal that different triggering level next pulse is launched;
C () draws the intensity of ion signal and the relation curve of triggering level according to the data obtained in previous step, to go forward side by side line linearity matching, according to the anti-peak area releasing ion signal when triggering level is zero of fitting result, namely obtain the intensity level of single ion signal.
The present invention makes ion gun to be measured with impulse form emitting ions by routine techniques means, and then is received by ion detector detection, on digital oscilloscope, finally obtain the signal peak of ion; Regulate the triggering level of digital oscilloscope, under each triggering level, all can obtain the signal intensity of ion gun institute's emitting ions in a pulse, namely obtain the relation of the ion signal intensity of a triggering level and an impulse ejection; Record the ion signal intensity level under multiple triggering level, draw corresponding image, just instead can release the signal intensity of single ion through linear fit.
The method of the invention is applicable to different ion guns to be measured, only need control ion gun to be measured with impulse form emitting ions.Described ion detector, accelerating field etc. are all ordinary skill in the art.Lorentz fit can improve the computational accuracy to signal peak area value.
Further, in step (b) under each triggering level to ion gun signal repetitive measurement, namely obtain the ion signal of the multiple pulses under each triggering level, and then average, as the intensity of the ion signal of the impulse ejection of under this triggering level.
Average and net result can be made more accurately reliable.
Further, ion gun is controlled in step (a) with nanosecond pulse emitting ions.
Nanosecond pulse can ensure that the amount of ions of each impulse ejection is few, and can ensure the time resolution of ion signal on time mass spectrum, so just can improve the degree of accuracy of measurement further.
The present invention adopts Lorentz fit and linear fit, and then the anti-signal intensity releasing single ion, and method therefor result is accurately reliable, and operation is very simple, can be applied to the detection to different kinds of ions source.
Accompanying drawing explanation
Fig. 1 measures the device schematic diagram of single ion signal in flight time mass spectrum.
1-vacuum chamber; 2-ionic pump; 3-ion gun to be measured; 4-accelerates aperture plate; 5-microchannel plate; 6-stainless steel electrode; 7-accelerates aperture plate power supply; 8-microchannel plate power supply; 9-digital delay pulse producer; 10-ion source controller; 11-digital oscilloscope; 12-pulse signal amplifier; 13-triggering level controller.
Fig. 2 flight time mass spectrum.Triggering level in figure is 8mV, and solid black lines is Lorentz fit, and in figure, data A is the area of peak-to-peak signal.
The relation of Fig. 3 ion signal integral area and triggering level.The matching of figure neutral line obtains area value 0.27V (4) the * ns with y-axis intersection point, namely corresponds to single Cs atom ion signal intensity.
Embodiment
The structural representation of equipment therefor when Fig. 1 is embody rule of the present invention.
Indicating 1 is a vacuum chamber, and pressure reaches 10
-3-10
-4pa.In this experiment, vacuum pressure can reach 10
-7pa, maintains vacuum tightness by ionic pump.The most basic structure of flight time mass spectrum in vacuum cavity: indicate 4 and be one and accelerate aperture plate, provide constant voltage by acceleration aperture plate power supply 7; Indicating 3 is ion guns to be measured, and this experiment uses the ion gun of alkali metal atom caesium.Indicating 5 is two pieces of microchannel plates, separates therebetween by the circular ring plate of thin stainless steel.In order to reduce the noise of detectable signal, the channel direction of microchannel plate is oppositely placed.Indicate the power supply that 8 are microchannel plate.Indicating 6 is one piece of stainless steel electrode (collector).Indicating 9 is digital delayed-pulse generators, can produce the nanosecond order even pulse control signal of picosecond magnitude.Indicating 10 is ion source controllers, for controlling ionogenic generation.Indicate 10 in this experiment and specifically adopt a pulsed dye laser, the light pulse that width is 8ns can be produced.Indicating 12 is pulse signal amplifiers, and its function is that the current signal of stainless steel electrode is converted into voltage signal, and amplifies.Indicating 11 is digital oscilloscopes.For recording and store the signal of flight time mass spectrum.Indicate the triggering level controller that 13 are digital oscilloscope.
During concrete detection, the control signal that digital delay pulse producer 9 produces nanosecond order is input to ion source controller 10, produces the light of nanosecond pulse, and then obtains the ion gun (indicating 3) of nanosecond pulse.Or by making acceleration aperture plate power supply 7 produce nanosecond pulse voltage, the ion gun of nanosecond pulse can be obtained equally.Ion gun accelerates to fly to ion detector (being made up of sign 5,6,8) under the effect accelerating the accelerating field that aperture plate 4 produces, and a large amount of electronics obtained through electron multiplication effect form electric current.By pulse signal amplifier 12, electric current is converted to voltage signal, and amplifies, finally pass into digital oscilloscope 11.
The first step: the triggering level regulating triggering level controller 13, can record the ion signal under different triggering level, obtain the integral area of current versus time through data processing on digital oscilloscope.Fig. 2 is triggering level when being set to 8mV, the flight time mass spectrum signal of the typical Cs atom ion of a width that digital oscilloscope collects.The depression of signal is darker, larger to represent the electron number after electron multiplication more for width.Owing to there is the electronic components such as electric capacity in collection signal circuit and amplification potential circuit, voltage signal is made to occur vibration.Utilize Lorentz fit can obtain the area value of peak-to-peak signal, the intensity of ion signal can be obtained.
Second step: the flight time mass spectrum measuring the Cs atom ion under a series of triggering level.Repetitive measurement under identical triggering level, averages, and draws the integral area (area value obtained after Lorentz fit) of ion signal and the relation of triggering level, carries out the area figures that linear fit obtains the intensity characterizing single ion signal.Fig. 3 is the result of test.The visible increase along with triggering level, the area of ion signal linearly increases.Carry out linear fit, the anti-area shifted onto when triggering level is zero is the quantificational expression of single ionic strength.
Illustrating: 1. when using the method for the invention to carry out isolated sub-ionization meter, ionogenic number should be made as far as possible few.2., when utilizing the method for the invention to carry out isolated sub-ionization meter on other devices, the change of partial devices, such as ion gun, ion detector, when amplifier etc. change, single ion area of acquisition is also different.But described device, especially method has versatility.Obtain isolated subsignal intensity and just can carry out quantitative test.
Claims (3)
1. measure a method for single ion signal in flight time mass spectrum, it is characterized in that, comprise the steps:
A () controls ion gun to be measured with impulse form emitting ions; The ion launched by ion gun to be measured is converted into corresponding current signal accelerate to fly to ion detector in vacuum environment under the effect of accelerating field after, be converted to corresponding voltage signal again, and amplify, finally input digital oscilloscope, obtain the ion signal being rendered as signal peak;
B () regulates the triggering level of digital oscilloscope, for each triggering level, Lorentz fit is utilized to obtain the area value of a corresponding signal peak encirclement, the namely intensity of the ion signal of an impulse ejection, and then the intensity obtaining the ion signal that different triggering level next pulse is launched;
C () draws the intensity of ion signal and the relation curve of triggering level according to the data obtained in previous step, to go forward side by side line linearity matching, according to the anti-peak area releasing ion signal when triggering level is zero of fitting result, namely obtain the intensity level of single ion signal.
2. a kind of method measuring single ion signal in flight time mass spectrum as claimed in claim 1, it is characterized in that, in step (b) under each triggering level to ion gun signal repetitive measurement, namely the ion signal of the multiple pulses under each triggering level is obtained, and then average, as the intensity of the ion signal of the impulse ejection of under this triggering level.
3. a kind of method measuring single ion signal in flight time mass spectrum as claimed in claim 1 or 2, is characterized in that, controls ion gun with nanosecond pulse emitting ions in step (a).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111856162A (en) * | 2020-07-10 | 2020-10-30 | 山西大学 | Vacuum air chamber electric field intensity measuring device and method based on time-of-flight mass spectrum |
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| CN1689134A (en) * | 2002-07-16 | 2005-10-26 | 力可公司 | Tandem time of flight mass spectrometer and method of use |
| WO2008080604A2 (en) * | 2006-12-29 | 2008-07-10 | Thermo Fisher Scientific (Bremen) Gmbh | Parallel mass analysis |
| CN102884608A (en) * | 2010-01-15 | 2013-01-16 | 莱克公司 | Ion trap mass spectrometer |
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Patent Citations (3)
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| CN1689134A (en) * | 2002-07-16 | 2005-10-26 | 力可公司 | Tandem time of flight mass spectrometer and method of use |
| WO2008080604A2 (en) * | 2006-12-29 | 2008-07-10 | Thermo Fisher Scientific (Bremen) Gmbh | Parallel mass analysis |
| CN102884608A (en) * | 2010-01-15 | 2013-01-16 | 莱克公司 | Ion trap mass spectrometer |
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| 元晋鹏 等: "飞行时间质谱探测磁光阱中超冷分子离子的实验研究", 《物理学报》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111856162A (en) * | 2020-07-10 | 2020-10-30 | 山西大学 | Vacuum air chamber electric field intensity measuring device and method based on time-of-flight mass spectrum |
| CN111856162B (en) * | 2020-07-10 | 2021-05-14 | 山西大学 | Vacuum air chamber electric field intensity measuring device and method based on time-of-flight mass spectrum |
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