CN101339160B - Plasma source ion synergic checking ion transfer spectrometer - Google Patents
Plasma source ion synergic checking ion transfer spectrometer Download PDFInfo
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- CN101339160B CN101339160B CN2008100225565A CN200810022556A CN101339160B CN 101339160 B CN101339160 B CN 101339160B CN 2008100225565 A CN2008100225565 A CN 2008100225565A CN 200810022556 A CN200810022556 A CN 200810022556A CN 101339160 B CN101339160 B CN 101339160B
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Abstract
The invention discloses a cooperative detection ion mobility spectrometer of the positive ion and negative ion of a plasma source; the plasma source has a positive metal electrode and a negative metal electrode, and voltage is imposed between the two electrodes so as to generate the plasma; the electrode is of the shape of a needle, rod, plate, cylinder or net, the discharging voltage is hundreds to thousands and the current is microampere to milliampere; the signal intensity of the ion source is large, the positive ion works cooperatively with the negative ion, therefore, the detection sensitivity is good, the resolution is high, the measurement speed is fast, the meter has small volume and simple operation and is applicable to fast online detection and alarming of trace amount of explosive, drugs and organic matters; compared with the radioactive source of the traditional ion mobility spectrometer, the plasma source has the advantage of no radioactivity, the spectrometer is convenient in use, maintenance and management and has high detection sensitivity and detection accuracy.
Description
Technical field:
The present invention relates to a kind of plasma source ion synergic checking ion transfer spectrometer, is to utilize that the migrate attribute of ion in electric field comes a kind of pick-up unit of separate substance under the atmospheric pressure.
Background technology:
Ion mobility spectrometry ion gun commonly used is a radioactive source
63Ni, its stable performance, volume be little, do not need additional power source, but because the use of radiomaterial; Make instrument aspect purchase, use, maintenance, management and disposal; To observe the radioactive source laws and regulations on the management, increase burden for users, limit the generally use of equipment.In addition,
63The ion number density that the Ni ion gun produces is certain, generally at a hundreds of pA, causes the detection sensitivity of Ni-IMS and dynamic range limited.The present invention uses plasma source, and the ion gun electric current is between μ A~mA, and ionic strength can improve the detection sensitivity of instrument far above the ionic strength that radioactive source produced, and the detection sensitivity of the ionic migration spectrometer that the present invention relates to can reach≤and 50 * 10
-12G.The ion flow of traditional in addition radioactive source can not change, and the ion gun among the present invention can carry out the adjusting of ion flow size as required.The plasma source that the present invention relates to is "dead", and human body is not had harm, is easy to use, maintenance and management and the marketing of instrument.
Ion mobility spectrometry needs the different working mode when different types of material is detected.Adopt negative ion during usually to explosive detection, adopt positive ion during to drugs and organism detection.Ionic migration spectrometer commonly used can only be worked under single ionic polarity, and instrument can not detect the explosive in the same sample, drugs and organism simultaneously.Ionic migration spectrometer among the present invention is the negative ions cooperative, can implement to detect simultaneously fast to the trace explosive in the sample, drugs and organism.
Summary of the invention:
The purpose of this invention is to provide a kind of new plasma source ion synergic checking ion transfer spectrometer; Produce plasma with atmosphere pressure discharging; Ion-molecule reaction between positive ion in the plasma or negative ion and the test substance is with substance ionization to be measured; By just/migration of negative ion in electric field separate to realize detecting in the test substance, is a kind of trace explosive, drugs and volatile organic matter device for fast detecting.
Technical scheme of the present invention:
A kind of high efficiency plasma body ion gun, the production method that it is characterized in that plasma source are between two metal electrodes of yin, yang, to apply voltage, form plasma; Electrode shape is pin, rod, plate, tube or netted, and to several kilovolts, electric current arrives a milliampere magnitude at microampere to sparking voltage at hundreds of; The polarity scalable of the signal intensity of plasma source, generation ion forms big positive ion and the negative ion of intensity, to satisfy the highly sensitive detection of trace explosive, drugs or volatile organic matter.
Plasma source ion synergic checking ion transfer spectrometer is characterized in that mainly being made up of plasma source, transference tube, gas purification driving, power supply part, acquisition of signal unit and embedded Control display; Plasma source is between two metal electrodes of yin, yang, to apply voltage, forms plasma; Electrode shape is pin, rod, plate, tube or netted, and to several kilovolts, electric current arrives a milliampere magnitude at microampere to sparking voltage at hundreds of; The polarity scalable of the signal intensity of plasma source, generation ion forms big positive ion and the negative ion of intensity, can carry out the negative ions cooperative, simultaneously explosive detection, drugs and organism.
Plasma source ion synergic checking ion transfer spectrometer structural drawing of the present invention is as shown in Figure 1, and test substance enters into reaction zone by injection port under carrier gas drives, and the reactive ion in the plasma source is with the measured matter ionization; The product ion that forms enters into the migration area; Arrive ion detector behind the motion certain hour and surveyed, handle, contrast of binding data storehouse and computing through software analysis; Last composition and the concentration that on display, provides measured matter, and can provide audible alarm.
Plasma source is used to produce the initial reaction ion, and when instrument was the positive ion detection mode, the key reaction ion was H
+(H
2O)
nWhen the negative ion working method, the key reaction ion is O
2 -(H
2O)
nPlasma ion source electrode structure provided by the invention can be pin, rod, plate, tube or netted; Negative electrode and anode are made up of metal material; Electrode distance is between mm~cm, and the electrode voltage that produces stable plasma arrives several kilovolts at hundreds of, and electric current arrives a milliampere magnitude at microampere.
The electric current that plasma source produces can be regulated through adjustable steady resistance.When the resistance of steady resistance was 50-100k Ω, the discharge current that produces between two electrodes was in μ A magnitude.When the resistance of steady resistance during at 10-100M Ω, two electric discharge between electrodes electric currents are in the mA magnitude.
The reactive ion R that ion gun produces
+/
-Under effect of electric field, entering into the reaction zone of migration tube, with the neutral test substance generation ion-molecule reaction that gets into reaction zone, is ion M with the measured matter molecular ionization
+/
-, when the ion gate in the migration tube was opened, ion entered into the migration Disengagement zone of migration tube; Migration tube is insulated the becket that interannular separates and is formed by a plurality of; Connect the identical resistance of resistance between the adjacent ring, after the migration tube two ends add certain voltage, in the migration Disengagement zone, form the electric field of a 200~400V/cm; Ion moves to detecting area under electric field action to be detected; Ion signal is sent into embedded system, compares through data processing and with database, obtains the kind and the concentration of the material of surveying.
The power supply unit that for ion synergic checking ion transfer spectrometer voltage is provided among the present invention is for develop high-voltage power supply voluntarily.The output voltage of power supply 0~± adjustable continuously in the 20.0kV scope, the adjusting of high pressure realizes by software, input D/A conversion+5V~-5V is corresponding+20~-regulation voltage of 20kV, the maximum current of power supply permission is 10mA.
When instrument carries out the positive ion detection; The migration tube initiating terminal is a positive high voltage; The ion mobility spectrometry figure that Fig. 2 obtains when being positive ion detection propionic aldehyde, Fig. 3 are the ion mobility spectrometry figure that obtains when detecting P-xylene, and Fig. 4 detects the migration spectrogram that obtains when being prone to system drugs acetone.When carrying out the negative ion detection, the migration tube initiating terminal is a negative high voltage, the migration spectrogram that obtains when Fig. 5 is negative ion explosive detection TNT (TNT).
The ionic migration spectrometer measuring principle
In ion mobility spectrometry, the reactive ion H that the ion source region produces
+(H
2O)
nOr O
2 -(H
2O)
nEnter into the ion-molecule reaction that reaction zone and measured matter M take place:
H
+(H
2O)
n+ M+X → MH
+(H
2O)
n *+ X (positive detecting pattern) (1)
O
2 -(H
2O)
n+ M+X → [MO
2 -(H
2O)
n]
*+ X (negative detecting pattern) (2)
The product ion that forms enters into the migration Disengagement zone of migration tube, under electric field action, makes travel motion.The migration velocity v of ion in electric field defers to rule:
v=KE (3)
Wherein, E is an electric field intensity, and K is an ion mobility, and its expression formula is:
In the formula, Z, e, be respectively ion with charge number and electron charge; N is the number density of neutral migration gas; μ is the reduced mass of ion m and migration gas molecule M; K is a Boltzmann constant; T is the temperature of migration gas; Ω is the collision cross-section of ionic molecule.
If the distance that ion moves in electric field is L, the used time is t, according to equation (3), then has:
Usually K is converted into the reduction mobility K under the standard conditions
0
Wherein, P is the observed pressure in the migration tube in the measuring process.In the instrument detecting, extract the quasi-molecular ions time of occurrence, calculate the reduction mobility by (5) and (6) formula, through with database comparison and calibration calculations, the kind and the concentration of coming definite material of surveying.
Advantage of the present invention:
Ion gun signal intensity of the present invention is big, just/and the negative ion collaborative work, so detection sensitivity is good, resolution is high, and measuring speed is fast, and the instrument volume is little, and is easy and simple to handle.Be applicable to trace explosive, drugs and organic quick online detection and warning.Compare with radioactive source in the traditional ion mobility spectrometry, the plasma source advantage is "dead", and instrument uses, maintenance and management is convenient, and detection sensitivity and detection accuracy height.
Description of drawings:
Fig. 1 is a plasma source ion synergic checking ion transfer spectrometer structural representation.
Fig. 2 is the ion mobility spectrometry figure of instrument detecting organism propionic aldehyde of the present invention.
Fig. 3 is the ion mobility spectrometry figure of instrument detecting organism P-xylene of the present invention.
Fig. 4 is that instrument of the present invention is surveyed the ion mobility spectrometry figure that is prone to system drugs acetone.
Fig. 5 is instrument detection of explosives TNT ion mobility spectrometry figure of the present invention.
Embodiment:
Referring to Fig. 1.
The difference of plasma source ion synergic checking ion transfer spectrometer and traditional ionic migration spectrometer is to use the ion gun of inactive plasma source as instrument, and can carry out positive and negative cooperative.Comprise transference tube, gas purification driver part, power supply part, acquisition of signal unit and data processing and display device.
Be example to measure explosive below, introduce the concrete detection mode of instrument.
At first use the tested article surface of sampling paper wiping; Sampling paper is sent to the injection port of instrument; Injection port heats sampling paper, will carry out high-temperature gasification attached to the explosive on sampling paper surface, and the explosive composition after the gasification is the reaction zone that enters into transference tube under the carrier gas of 300mL/min drives at flow; Surveyed by ionization and through arriving last detector behind the Disengagement zone; Amplifier in the detecting area is a voltage signal with the ion flow conversion of signals on the ion detection plate, and conversion converts analog voltage signal into digital signal through A/D, and is transferred to the data analysis part; Signal is analyzed; In conjunction with gas temperature, pressure and other parameters, through with set up in advance comprise explosive amount of ions, kind, the database of mobility compares and through related operation separately, and and explosive ionic strength-concentration between the calculating of demarcation relation; Obtain final testing result, final ion signal spectrogram is shown by the color LCD LCDs at terminal and provides alerting signal.
Claims (1)
1. plasma source ion synergic checking ion transfer spectrometer is characterized in that: mainly be made up of plasma source, transference tube, gas purification driving, power supply part, acquisition of signal unit and embedded Control display;
Said plasma source is between two metal electrodes of yin, yang, to apply voltage, forms plasma; Electrode shape is pin, rod, plate, tube or netted; The polarity scalable of the ionic strength of plasma source, generation ion: sparking voltage arrives several kilovolts at hundreds of; Electric current arrives a milliampere magnitude at microampere; So that form big positive ion and the negative ion of intensity, can carry out the cooperative of negative ions, thus while explosive detection, drugs and organism;
The reactive ion R that said plasma source produces
+/
-Under effect of electric field, entering into the reaction zone of migration tube, with the neutral test substance that gets into reaction zone ion-molecule reaction takes place directly, is ion M with the measured matter molecular ionization
+/
-, when the ion gate in the migration tube was opened, ion entered into the migration Disengagement zone of migration tube; Migration tube is insulated the becket that interannular separates and is formed by a plurality of; Connect the identical resistance of resistance between the adjacent ring, after the migration tube two ends add certain voltage, in the migration Disengagement zone, form the electric field of a 200~400V/cm; Ion moves to detecting area under electric field action to be detected; Ion signal is sent into embedded system, compares through data processing and with database, obtains the kind and the concentration of the material of surveying;
Said power supply part is that ion synergic checking ion transfer spectrometer provides voltage; Wherein, in the said power supply part output voltage of power supply 0~± adjustable continuously in the 20.0kV scope, the adjusting of high pressure realizes by software, input D/A conversion+5V~-5V is corresponding+20~-regulation voltage of 20kV, the maximum current of power supply permission is 10mA;
Further, said data processing and with database relatively, the process of kind and concentration that obtains the material of surveying is following:
In ion mobility spectrometry, the positive reaction IONS OF H that the ion source region produces
+(H
2O)
nOr negative reaction ion O
2 -(H
2O)
nUnder the respective detection pattern, enter into reaction zone, the ion-molecule reaction that takes place with measured matter M respectively:
H
+(H
2O)
n+ M+X → MH
+(H
2O)
n *The positive detecting pattern of+X (1)
O
2 -(H
2O)
n+ M+X → [MO
2 -(H
2O)
n]
*+ X bears detecting pattern (2)
The product ion that forms enters into the migration Disengagement zone of migration tube, under electric field action, makes travel motion; The migration velocity v of ion in electric field defers to rule:
v=KE (3)
Wherein, E is an electric field intensity, and K is an ion mobility, and its expression formula is:
Wherein,
Z, e, be respectively ion with charge number and electron charge; N is the number density of neutral migration gas; μ is the reduced mass of ion m and migration gas molecule M; K is a Boltzmann constant; T is the temperature of migration gas; Ω is the collision cross-section of ionic molecule;
If the distance that ion moves in electric field is L, the used time is t, according to equation (3), then has:
Usually K is converted into the reduction mobility K under the standard conditions
0:
Wherein, P is the observed pressure in the migration tube in the measuring process; In the instrument detecting, extract the quasi-molecular ions time of occurrence, calculate the reduction mobility by (5) and (6) formula, through with database comparison and calibration calculations, the concrete kind and the concentration of coming definite material of surveying.
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Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101937823B (en) * | 2009-06-30 | 2012-05-23 | 同方威视技术股份有限公司 | Ion collecting device of ion mobility spectrometer and ion mobility spectrometer |
CN102313774B (en) * | 2010-06-30 | 2013-05-08 | 清华大学 | Ion gate structure and operation method of ionic migration spectrometer |
CN101949889B (en) * | 2010-08-10 | 2012-10-17 | 公安部第三研究所 | Drug explosive ion mobility spectrum detection device |
CN102479663A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Ion mobility tube and applications thereof |
CN102568974A (en) * | 2012-01-12 | 2012-07-11 | 北京交通大学 | Discharging electrode and plasma generating device utilizing same |
CN102548176A (en) * | 2012-01-12 | 2012-07-04 | 北京交通大学 | Discharge electrode and plasma generating device using same |
CN103871827A (en) * | 2012-12-12 | 2014-06-18 | 中国科学院大连化学物理研究所 | Crossing type ion migration tube |
CN103245719A (en) * | 2013-05-09 | 2013-08-14 | 河北工程大学 | Rapid detector for trace aniline in drinking water |
CN103364480B (en) * | 2013-07-11 | 2015-07-15 | 中国船舶重工集团公司第七一八研究所 | Detection system for IMS (Ion Mobility Spectrometry) explosives |
CN104465297B (en) * | 2013-09-16 | 2017-02-22 | 中国科学院大连化学物理研究所 | Gas control method of parallel double-ion migration tube |
CN103635004A (en) * | 2013-12-13 | 2014-03-12 | 南开大学 | Method for measuring ion species and number density distribution of plasma |
CN105954350A (en) * | 2016-06-03 | 2016-09-21 | 河北工程大学 | Gas phase ion molecule collision cross section measuring instrument and collision cross section measuring method at atmospheric pressure |
CN111208189A (en) * | 2018-11-21 | 2020-05-29 | 中国科学院大连化学物理研究所 | Method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions |
CN111220687A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Ion mobility spectrometer with built-in sample introduction region |
CN111220688A (en) * | 2018-11-26 | 2020-06-02 | 中国科学院大连化学物理研究所 | Ion mobility spectrometer with solid-liquid-gas sampling device |
CN112697870A (en) * | 2020-12-02 | 2021-04-23 | 深圳市鑫源通电子有限公司 | Detector for narcotic drugs without radioactive source explosive |
CN114007321A (en) * | 2021-09-30 | 2022-02-01 | 中科等离子体科技(合肥)有限公司 | Diagnosis method for electron density of atmospheric pressure plasma |
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Non-Patent Citations (2)
Title |
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