CN111208189A - Method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions - Google Patents
Method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions Download PDFInfo
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- CN111208189A CN111208189A CN201811387774.9A CN201811387774A CN111208189A CN 111208189 A CN111208189 A CN 111208189A CN 201811387774 A CN201811387774 A CN 201811387774A CN 111208189 A CN111208189 A CN 111208189A
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Abstract
The method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions comprises the following steps: 1) respectively preparing standard sample solutions of known explosives and drugs; 2) establishing a standard sample reduced mobility database; testing of the actual samples: and (3) wiping the surface of the target to be detected by using a sampling sheet to sample or sampling by dripping a solution containing the target to be detected on the sampling sheet, respectively obtaining spectrograms or reduction mobility rates in a positive ion mode and a negative ion mode by single sample introduction according to the process of the step 2), and comparing the spectrograms or reduction mobility rates with the spectrograms or reduction mobility rates of the known explosives and the drugs obtained in the step 2) one by one.
Description
Technical Field
A method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions belongs to the field of analytical instruments and relates to a method for qualitative and quantitative analysis of novel peroxide explosives, traditional explosives and drugs. The problem that the single-mode measurement range of the traditional single ion mobility tube is limited is overcome; the problems that the two migration tubes are large in size and power consumption and sensitivity is reduced due to shunting are solved. The invention provides scientific reference for comprehensive qualitative and quantitative analysis of explosives and drugs.
Background
At present, terrorism is rampant increasingly and seriously threatens the life and property safety of people. In recent years, terrorist activities in China are also in a remarkable growth situation, and malignant cases frequently occur. Particularly, terrorist reflux becomes a new anti-terrorist characteristic along with the increase of the international terrorist force. And through the training of foreign terrorists, the preparation method of explosives is mastered by reflux terrorists. The chances of an explosive event occurring are dramatically increased. Therefore, it is highly desirable if the concealed explosives can be detected quickly and accurately.
The detection method of the explosive mainly comprises ion mobility spectrometry, an X-ray machine, terahertz, a chromatograph, a Raman spectrometer, an infrared spectrometer and the like. Among them, ion mobility spectrometry is the mainstream means of the field detection of trace explosives at present. Principle of ion mobility spectrometry: the sample vapor or particles to be detected are firstly gasified and then carried into the reaction area of the drift tube by the carrier gas. Within the reaction zone, the sample gas is first ionized to form product ions. The switching pulses controlling the ion gate constitute ion sheets that periodically enter the drift region. Under the action of the drift electric field, the product ions fly to the Faraday chassis along the axial direction. The mobility of the ions depends on the mass, structure, etc. of the ions. The product ions generated by different substances have different mobility under the same electric field, so the drift time used for passing through the whole drift region length is different, thereby identifying the variety of the detected object. With the advent of new peroxide explosives, traditional single anion mode detection has not been able to meet the demand. For this reason, development of detection modes of both positive and negative modes is required. Patent one (patent No. 200910265443.2) reports a bipolar ion mobility tube, in which two reaction regions and two mobility regions are coaxial, and positive and negative high voltages are applied respectively to realize detection of positive and negative ions. Patent two (patent No. 201310422399.8) reports a parallel dual-ion migration tube, which uses two migration tubes to respectively realize positive and negative ion detection. Both of them achieve positive and negative ion detection, but two migration tubes or two migration zones increase volume and power consumption undoubtedly.
The application provides a method for simultaneously measuring explosives and drugs by using an ion mobility spectrometry based on rapid switching of positive ions and negative ions. Through fast switch over, realize just, the multiple switch over of two kinds of modes of burden in the sample thermal desorption cycle of single appearance of feeding, obtain the enough information of novel peroxide explosive and traditional explosive and drugs, realize comprehensive accurate detection.
Disclosure of Invention
The method for measuring explosives and drugs by fast switching ion mobility spectrometry of positive ions and negative ions comprises the following steps:
1) preparing standard sample solutions of known explosives and drugs respectively: acetone, methanol, acetonitrile or a mixture of methanol and acetonitrile are taken as solvents, and then the volume is fixed to a certain volume to prepare standard sample solutions of known explosives and drugs respectively;
2) and establishing a standard sample reduced mobility database: taking an ion mobility spectrometry capable of rapidly switching positive and negative ion detection modes as a detection instrument, respectively dropping known explosive and drug standard sample solutions on a sampling sheet, putting a thermal analysis sample injector after solvent evaporation is finished, performing thermal analysis, performing ion mobility spectrometry, respectively obtaining corresponding spectrograms of the known explosive and drug standard sample solutions in a positive ion mode and a negative ion mode by single sample injection, and establishing spectrograms or reduced mobility databases of the known explosive and drug standard sample solutions;
the ion mobility spectrometry with the positive and negative ion detection modes capable of being rapidly switched refers to that a direct-current power supply capable of alternately outputting positive high voltage and negative high voltage is adopted as an electric field control power supply of an ion mobility spectrometry reaction area and a migration area, and the direct-current power supply outputs square wave voltage;
testing of the actual samples: the surface of a target to be detected is wiped by using a sampling sheet for sampling or the surface of the target to be detected is sampled in a manner of dripping a solution containing the target to be detected on the sampling sheet, spectrograms or reduced mobility in a positive ion mode and a negative ion mode are respectively obtained by single sample injection according to the process of the step 2), the spectrograms or the reduced mobility are compared with the spectrograms or the reduced mobility of the known explosives and the drugs obtained in the step 2) one by one, whether the same spectrograms or the reduced mobility exist or not is searched, then a qualitative detection result can be given, the target to be detected has the same spectrogram or the reduced mobility, namely the target to be detected is the corresponding known explosives or drugs, and the target to be detected does not have the same spectrogram or the reduced mobility, namely the target to be detected is not in the known explosives or drugs in.
In the method, in the ion mobility spectrometry detection process of explosives or drugs, the detection mode of the ion mobility spectrometry is rapidly switched between a positive ion mode and a negative ion mode, the detection of peroxide explosives or drugs is realized in the positive ion mode, the detection of traditional nitro explosives is realized in the negative ion mode, and the analysis of explosives and drugs in single sample injection is realized through rapid switching;
the detection mode of the ion mobility spectrometry can be a positive ion detection mode firstly and then switched to a negative ion detection mode; the time of the positive and negative ion detection modes may be the same or may be different.
According to the method, the detection mode of the ion mobility spectrometry is firstly carried out in a negative ion detection mode, and then the detection mode is switched to a positive and negative ion detection mode; the time of the positive and negative ion detection modes may be the same or may be different.
According to the method, the switching frequency of the positive ion mode and the negative ion mode is higher than 0.01 Hz.
According to the method, explosives which can be detected in a positive ion mode comprise peroxide explosives such as TATP or HMTD, or opium, heroin, morphine, hemp, cocaine, methamphetamine, K powder (ketamine) or amphetamine;
the explosives which can be detected in the negative ion mode comprise one of various military explosives, civil explosives and earthen explosives; such as TNT, hexogen (RDX), octogen (HMX), Taian (PETN), nitroglycerin, ammonium nitrates, gunpowder, plastic explosives (C3, C4), picric acid, or troxer.
The method is characterized in that the known explosives and drugs are as follows: TATP, HMTD, opium, heroin, morphine, cannabis, cocaine, methamphetamine, K powder (ketamine) amphetamine, TNT, hexogen (RDX), octogen (HMX), taian (PETN), nitroglycerin, nitramines, gunpowder, plastic explosives (C3, C4), picric acid, or terbutaline.
Drawings
Fig. 1 is a typical spectrum of a reactive ion at fast switching.
FIG. 2 is a detection spectrum of TNT and TATP.
Detailed Description
The voltage of the high-voltage power supply capable of being rapidly switched is a square wave power supply with the amplitude of 5kV, and the switching frequency is 50 Hz. The ionization source is a VUV ionization source, and the reagent molecules are 100ppm acetone. The samples were TNT and TATP standard solutions and the solvent was acetone. The length of the migration zone was 5cm and the length of the reaction zone was 3 cm. Figure 1 shows a typical spectrum of the reactive ion at fast switching. The corresponding peak-off times are 4ms and 3ms, respectively. Respectively dripping 1uL of TATP with the concentration of 200ng/uL and 1uL of TNT with the concentration of 5ng/uL on a tetrafluoro sampling sheet, putting the sampling sheet into a thermal desorption sample injector to desorb and gasify after no obvious acetone solvent exists on the tetrafluoro sampling sheet, and then entering ion mobility spectrometry detection. FIG. 2 shows the detection spectra of TNT and TATP, the TATP peak at 3.65ms in positive ion mode; and the two peak positions of TNT in negative ion mode are 4.7 and 4.9ms, respectively.
Claims (6)
1. The method for measuring explosives and drugs by fast switching of positive ions and negative ions is characterized by comprising the following steps of:
1) preparing standard sample solutions of known explosives and drugs respectively: acetone, methanol, acetonitrile or a mixture of methanol and acetonitrile are taken as solvents, and then the volume is fixed to a certain volume to prepare standard sample solutions of known explosives and drugs respectively;
2) and establishing a standard sample reduced mobility database: taking an ion mobility spectrometry capable of rapidly switching positive and negative ion detection modes as a detection instrument, respectively dropping known explosive and drug standard sample solutions on a sampling sheet, putting a thermal analysis sample injector after solvent evaporation is finished, performing thermal analysis, performing ion mobility spectrometry, respectively obtaining corresponding spectrograms of the known explosive and drug standard sample solutions in a positive ion mode and a negative ion mode by single sample injection, and establishing spectrograms or reduced mobility databases of the known explosive and drug standard sample solutions;
the ion mobility spectrometry with the positive and negative ion detection modes capable of being rapidly switched refers to that a direct-current power supply capable of alternately outputting positive high voltage and negative high voltage is adopted as an electric field control power supply of an ion mobility spectrometry reaction area and a migration area, and the direct-current power supply outputs square wave voltage;
3) and testing of the actual sample: the surface of a target to be detected is wiped by using a sampling sheet for sampling or the surface of the target to be detected is sampled in a manner of dripping a solution containing the target to be detected on the sampling sheet, spectrograms or reduced mobility in a positive ion mode and a negative ion mode are respectively obtained by single sample injection according to the process of the step 2), the spectrograms or the reduced mobility are compared with the spectrograms or the reduced mobility of the known explosives and the drugs obtained in the step 2) one by one, whether the same spectrograms or the reduced mobility exist or not is searched, then a qualitative detection result can be given, the target to be detected has the same spectrogram or the reduced mobility, namely the target to be detected is the corresponding known explosives or drugs, and the target to be detected does not have the same spectrogram or the reduced mobility, namely the target to be detected is not in the known explosives or drugs in.
2. The method of claim 1, wherein:
in the ion mobility spectrometry detection process of explosives or drugs, the detection mode of the ion mobility spectrometry is rapidly switched between a positive ion mode and a negative ion mode, the detection of peroxide explosives or drugs is realized in the positive ion mode, the detection of traditional nitro explosives is realized in the negative ion mode, and the analysis of single sample injection explosives and drugs is realized through rapid switching;
the detection mode of the ion mobility spectrometry can be a positive ion detection mode firstly and then switched to a negative ion detection mode; the time of the positive and negative ion detection modes may be the same or may be different.
3. The method of claim 1, wherein:
the detection mode of the ion mobility spectrometry is firstly carried out in a negative ion detection mode, and then the detection mode is switched to a positive and negative ion detection mode; the time of the positive and negative ion detection modes may be the same or may be different.
4. A method according to claim 1, 2 or 3, characterized in that:
the switching frequency of the positive ion mode and the negative ion mode is higher than 0.01 Hz.
5. The method of claim 1, wherein:
explosives which can be detected in positive ion mode include peroxide explosives such as TATP or HMTD, or opium, heroin, morphine, hemp, cocaine, methamphetamine, K powder (ketamine) or amphetamine;
the explosives which can be detected in the negative ion mode comprise one of various military explosives, civil explosives and earthen explosives; such as TNT, hexogen (RDX), octogen (HMX), TAIAN (PETN), nitroglycerin, ammonium nitrates, black powder, plastic explosives (C3, C4), picric acid, or troxer.
6. The method of claim 1, wherein:
explosives and drugs are known as: TATP, HMTD, opium, heroin, morphine, cannabis, cocaine, methamphetamine, K powder (ketamine) amphetamine, TNT, hexogen (RDX), octogen (HMX), taian (PETN), nitroglycerin, nitramines, gunpowder, plastic explosives (C3, C4), picric acid, or terbutaline.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112098502A (en) * | 2020-09-15 | 2020-12-18 | 中国科学院空天信息创新研究院 | Detection method for calibrating ion mobility spectrometer by utilizing multiple ion peaks |
| CN114088802A (en) * | 2021-12-15 | 2022-02-25 | 中国科学院大连化学物理研究所 | Single-tube positive-negative dual-mode fast switching ion mobility spectrometry and working time sequence |
Citations (2)
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| CN101339160A (en) * | 2008-08-15 | 2009-01-07 | 中国科学院安徽光学精密机械研究所 | Plasma source ion synergic checking ion transfer spectrometer |
| CN101949889A (en) * | 2010-08-10 | 2011-01-19 | 公安部第三研究所 | Drug explosive ion mobility spectrum detection device |
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2018
- 2018-11-21 CN CN201811387774.9A patent/CN111208189A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101339160A (en) * | 2008-08-15 | 2009-01-07 | 中国科学院安徽光学精密机械研究所 | Plasma source ion synergic checking ion transfer spectrometer |
| CN101949889A (en) * | 2010-08-10 | 2011-01-19 | 公安部第三研究所 | Drug explosive ion mobility spectrum detection device |
Non-Patent Citations (3)
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| 吕勇杰: "离子迁移谱技术及其在毒品和爆炸物检测中的应用", 《中国优秀硕士学位论文全文数据库社会科学Ⅰ辑》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112098502A (en) * | 2020-09-15 | 2020-12-18 | 中国科学院空天信息创新研究院 | Detection method for calibrating ion mobility spectrometer by utilizing multiple ion peaks |
| CN112098502B (en) * | 2020-09-15 | 2023-04-18 | 中国科学院空天信息创新研究院 | Detection method for calibrating ion mobility spectrometer by utilizing multiple ion peaks |
| CN114088802A (en) * | 2021-12-15 | 2022-02-25 | 中国科学院大连化学物理研究所 | Single-tube positive-negative dual-mode fast switching ion mobility spectrometry and working time sequence |
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