CN104713941B - A kind of organic and inorganic comprehensive analyzer of explosive - Google Patents
A kind of organic and inorganic comprehensive analyzer of explosive Download PDFInfo
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- CN104713941B CN104713941B CN201310690977.6A CN201310690977A CN104713941B CN 104713941 B CN104713941 B CN 104713941B CN 201310690977 A CN201310690977 A CN 201310690977A CN 104713941 B CN104713941 B CN 104713941B
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- 239000002360 explosive Substances 0.000 title claims abstract description 47
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000007789 gas Substances 0.000 claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- 239000012159 carrier gas Substances 0.000 claims abstract description 23
- 239000004744 fabric Substances 0.000 claims abstract description 13
- 238000005070 sampling Methods 0.000 claims abstract description 13
- 238000003795 desorption Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001871 ion mobility spectroscopy Methods 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims 1
- 238000002076 thermal analysis method Methods 0.000 abstract description 20
- 238000001514 detection method Methods 0.000 abstract description 14
- 150000002500 ions Chemical class 0.000 abstract description 10
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 239000002019 doping agent Substances 0.000 abstract description 4
- 238000004949 mass spectrometry Methods 0.000 abstract 1
- 239000012070 reactive reagent Substances 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000004451 qualitative analysis Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 238000005040 ion trap Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- OXZOLXJZTSUDOM-UHFFFAOYSA-N fluoro 2,2,2-trifluoroacetate Chemical class FOC(=O)C(F)(F)F OXZOLXJZTSUDOM-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及质谱分析仪器，具体的说是一种有机和无机爆炸物全面分析仪，包括热解析进样器、采样布、镍源、低温等离子体电离源和分析器，于热解析进样器上设置有载气入口和样品气出口；采样布置于热解析进样器内，采样布上的样品经热解析后进样；于热解析进样器的样品气出口后端的气路上依次设置有镍源、低温等离子体电离源和分析器。本发明的爆炸物全面分析仪，通过低温等离子体电离源和镍源两种电离方式，可全面检测有机和无机爆炸物；对于两种电离源都能电离的爆炸物，还能提高电离效率和检测灵敏度；在载气或者低温等离子体电离源的放电气体中添加掺杂气体，可改变电离源中的反应试剂离子，提高爆炸物检测的选择性和特异性。The invention relates to a mass spectrometry instrument, specifically a comprehensive analyzer for organic and inorganic explosives, comprising a thermal analysis sampler, a sampling cloth, a nickel source, a low-temperature plasma ionization source and an analyzer, and a thermal analysis sampler There is a carrier gas inlet and a sample gas outlet on the top; the sampling is arranged in the thermal analysis sampler, and the sample on the sampling cloth is injected after thermal analysis; the gas path at the rear end of the sample gas outlet of the thermal analysis sampler Nickel source, low temperature plasma ionization source and analyzer. The comprehensive analyzer for explosives of the present invention can fully detect organic and inorganic explosives through two ionization modes of low-temperature plasma ionization source and nickel source; for explosives that can be ionized by both ionization sources, the ionization efficiency and Detection sensitivity; adding dopant gas to the carrier gas or the discharge gas of the low-temperature plasma ionization source can change the reactive reagent ions in the ionization source and improve the selectivity and specificity of explosive detection.
Description
技术领域technical field
本发明涉及质谱分析仪器，具体的说是一种有机和无机爆炸物全面分析仪。本发明通过低温等离子体电离源和镍源两种电离方式，可以全面检测有机和无机爆炸物；对于两种电离源都能电离的爆炸物，可以提高电离效率和检测灵敏度；在载气或者低温等离子体电离源的放电气体中添加掺杂气体，可以改变电离源中的反应试剂离子，提高爆炸物检测的选择性和特异性，有利于爆炸物的定性分析。The invention relates to a mass spectrum analysis instrument, in particular to a comprehensive analyzer for organic and inorganic explosives. The invention can comprehensively detect organic and inorganic explosives through two ionization methods of low-temperature plasma ionization source and nickel source; for explosives that can be ionized by both ionization sources, the ionization efficiency and detection sensitivity can be improved; Adding dopant gas to the discharge gas of the plasma ionization source can change the reagent ions in the ionization source, improve the selectivity and specificity of explosive detection, and facilitate the qualitative analysis of explosives.
背景技术Background technique
低温等离子体电离源基于介质阻挡放电原理，利用He、Ar、N2、空气等作为放电气体，在玻璃管的内、外两个电极上施加射频电压就能发生介质阻挡放电，产生低温等离子体，利用低温等离子体可以电离样品。低温等离子体电离源已经应用于检测爆炸物，表现出高灵敏和无需样品前处理，直接电离复杂基质中的爆炸物，并且可以直接电离绝缘体以及导体表面上的爆炸物等优越的性能。在低温等离子体电离源的放电气体中添加反应试剂气体如卤代烷烃和四氟乙酸等，还能形成新的爆炸物产物离子，提高爆炸物检测的选择性和特异性，有利于爆炸物的定性分析。但是，低温等离子体电离源主要应用于电离有机爆炸物，不能电离无机爆炸物或者电离无机爆炸物时电离效率较低。The low-temperature plasma ionization source is based on the principle of dielectric barrier discharge, using He, Ar, N 2 , air, etc. as the discharge gas, and applying radio frequency voltage to the inner and outer electrodes of the glass tube to generate dielectric barrier discharge and low-temperature plasma , samples can be ionized using low-temperature plasma. The low-temperature plasma ionization source has been applied to the detection of explosives, showing high sensitivity, no need for sample pretreatment, direct ionization of explosives in complex matrices, and direct ionization of explosives on the surface of insulators and conductors. Adding reaction reagent gases such as halogenated alkanes and tetrafluoroacetic acid to the discharge gas of the low-temperature plasma ionization source can also form new explosive product ions, improve the selectivity and specificity of explosive detection, and facilitate the qualitative identification of explosives analyze. However, the low-temperature plasma ionization source is mainly used to ionize organic explosives, and the ionization efficiency is low when it cannot ionize inorganic explosives or ionize inorganic explosives.
镍源是一种高灵敏、高稳定性的电离源。镍源作为离子迁移谱的常用电离源，已经广泛应用于爆炸物的检测中，并且非常适合用于电离无机爆炸物。采用镍源电离爆炸物时，在样品载气如空气中添加掺杂气体如二氯甲烷、O3等，可以改变镍源中的反应试剂离子，得到不同的爆炸物产物离子，进而提高爆炸物检测的特异性和灵敏度，有利于爆炸物的定性分析。The nickel source is a highly sensitive and stable ionization source. As a common ionization source for ion mobility spectrometry, nickel source has been widely used in the detection of explosives and is very suitable for ionizing inorganic explosives. When a nickel source is used to ionize explosives, adding doping gases such as dichloromethane, O 3 , etc. to the sample carrier gas such as air can change the reagent ions in the nickel source to obtain different explosive product ions, thereby increasing the concentration of explosives. The specificity and sensitivity of detection are beneficial to the qualitative analysis of explosives.
由此，本发明设计了一种有机和无机爆炸物全面分析仪，通过低温等离子体电离源和镍源两种电离方式，可以全面检测有机和无机爆炸物；对于两种电离源都能电离的爆炸物，可以提高电离效率和检测灵敏度；在载气或者低温等离子体电离源的放电气体中添加掺杂气体，可以改变电离源中的反应试剂离子，提高爆炸物检测的选择性和特异性，有利于爆炸物的定性分析。Therefore, the present invention has designed a kind of organic and inorganic explosive comprehensive analyzer, can detect organic and inorganic explosive comprehensively through two kinds of ionization modes of low temperature plasma ionization source and nickel source; Can ionize for two kinds of ionization sources Explosives can improve the ionization efficiency and detection sensitivity; adding dopant gas to the discharge gas of the carrier gas or low-temperature plasma ionization source can change the reaction reagent ions in the ionization source and improve the selectivity and specificity of explosive detection. Conducive to the qualitative analysis of explosives.
发明内容Contents of the invention
本发明的目的在于提供一种有机和无机爆炸物全面分析仪。The object of the present invention is to provide a comprehensive analyzer for organic and inorganic explosives.
为实现上述目的，本发明采用的技术方案为：To achieve the above object, the technical solution adopted in the present invention is:
一种有机和无机爆炸物全面分析仪，包括热解析进样器、采样布、镍源、低温等离子体电离源和分析器，于热解析进样器上设置有载气入口和样品气出口；A comprehensive analyzer for organic and inorganic explosives, including a thermal desorption sampler, a sampling cloth, a nickel source, a low-temperature plasma ionization source and an analyzer. The thermal desorption sampler is provided with a carrier gas inlet and a sample gas outlet;
采样布置于热解析进样器内，采样布上的样品经热解析后进样；The sampling is arranged in the thermal analysis injector, and the sample on the sampling cloth is injected after thermal analysis;
载气从热解析进样器的载气入口流入，载带样品分子从样品气出口流出；于热解析进样器的样品气出口后端的气路上设置有镍源；于镍源后端的气路上设置有低温等离子体电离源；于低温等离子体电离源后端的气路上设置有分析器。The carrier gas flows in from the carrier gas inlet of the thermal analysis sampler, and the carrier sample molecules flow out from the sample gas outlet; a nickel source is set on the gas path at the rear end of the sample gas outlet of the thermal analysis sampler; the gas path at the rear end of the nickel source A low-temperature plasma ionization source is provided; an analyzer is provided on the gas path at the back end of the low-temperature plasma ionization source.
热解析进样器通过热金属块对样品进行接触加热，或者通过加热灯对样品进行非接触加热。The thermal desorption sampler heats the sample through a hot metal block, or heats the sample non-contact through a heating lamp.
所述的载气为空气或者氮气中的一种或者为两种气体的混合气。The carrier gas is one of air or nitrogen or a mixture of the two gases.
从热解析进样器热解析出来的样品分子经镍源和低温等离子体电离源电离后流入分析器进行分析；所述的分析器为质谱分析器或者离子迁移谱。The sample molecules thermally desorbed from the thermal desorption sampler are ionized by a nickel source and a low-temperature plasma ionization source, and then flow into an analyzer for analysis; the analyzer is a mass spectrometer or an ion mobility spectrometer.
本发明的有益效果在于：本发明设计的有机和无机爆炸物全面分析仪，通过低温等离子体电离源和镍源两种电离方式，可以全面检测有机和无机爆炸物；对于两种电离源都能电离的爆炸物，可以提高电离效率和检测灵敏度；在载气或者低温等离子体电离源的放电气体中添加掺杂气体，可以改变电离源中的反应试剂离子，提高爆炸物检测的选择性和特异性，有利于爆炸物的定性分析。The beneficial effects of the present invention are that: the organic and inorganic explosives comprehensive analyzer designed by the present invention can fully detect organic and inorganic explosives through two ionization modes of low-temperature plasma ionization source and nickel source; Ionized explosives can improve ionization efficiency and detection sensitivity; adding dopant gas to the discharge gas of the carrier gas or low-temperature plasma ionization source can change the reagent ions in the ionization source and improve the selectivity and specificity of explosive detection It is beneficial to the qualitative analysis of explosives.
附图说明Description of drawings
图1为本发明的有机和无机爆炸物全面分析仪的结构示意图。Fig. 1 is the structure schematic diagram of organic and inorganic explosive comprehensive analyzer of the present invention.
其中，1-热解析进样器；2-载气入口；3-样品气出口；4-采样布；5-镍源；6-低温等离子体电离源；7-分析器。Among them, 1-thermal desorption sampler; 2-carrier gas inlet; 3-sample gas outlet; 4-sampling cloth; 5-nickel source; 6-low temperature plasma ionization source; 7-analyzer.
具体实施方式detailed description
如图1所示，一种有机和无机爆炸物全面分析仪，包括热解析进样器1、采样布4、镍源5、低温等离子体电离源6和分析器7，于热解析进样器1上设置有载气入口2和样品气出口3；As shown in Figure 1, a kind of organic and inorganic explosives comprehensive analyzer comprises thermal desorption sample injector 1, sampling cloth 4, nickel source 5, low temperature plasma ionization source 6 and analyzer 7, in thermal desorption sample injector 1 is provided with a carrier gas inlet 2 and a sample gas outlet 3;
采样布4置于热解析进样器1内，采样布4的材料为聚四氟乙烯，采样布4上的爆炸物样品经热解析后进样；Sampling cloth 4 is placed in thermal analysis injector 1, and the material of sampling cloth 4 is polytetrafluoroethylene, and the explosive sample on sampling cloth 4 is injected after thermal analysis;
实施例1Example 1
热解析进样器1通过卤素光束加热灯LCB-50对样品进行非接触加热，加热灯与采样布4之间的距离为35mm。The thermal analysis sampler 1 uses the halogen beam heating lamp LCB-50 to heat the sample non-contact, and the distance between the heating lamp and the sampling cloth 4 is 35 mm.
载气从热解析进样器1的载气入口2流入，载带样品分子从样品气出口3流出；载气为纯净的干燥空气，载气流速为100-500mL/min。The carrier gas flows in from the carrier gas inlet 2 of the thermal analysis injector 1, and the sample molecules flow out from the sample gas outlet 3; the carrier gas is pure dry air, and the carrier gas flow rate is 100-500mL/min.
于热解析进样器1的样品气出口3后端的气路上设置有镍源5；镍源5与样品气出口3的距离为15mm。A nickel source 5 is provided on the gas path at the rear end of the sample gas outlet 3 of the thermal analysis injector 1; the distance between the nickel source 5 and the sample gas outlet 3 is 15 mm.
于镍源5后端的气路上设置有低温等离子体电离源6；低温等离子体电离源6与镍源5的距离为10mm。低温等离子体电离源6采用外径为6mm、厚为1mm的玻璃管作为介质，玻璃管外套有内径为6.1mm、厚为0.1mm、长为16mm的不锈钢圆筒作为射频高压电极，玻璃管内有外径为1.58mm、长为100mm的金属圆柱杆作为地电极，在两电极之间施加频率为25KHz，峰峰值为2KVp-p的射频电压；放电气体为He气，流量为0.2-1L/min；可以选择在He气中添加二氯甲烷、水蒸气等掺杂气体，提高爆炸物检测的特异性和灵敏度。A low-temperature plasma ionization source 6 is arranged on the gas path at the rear end of the nickel source 5; the distance between the low-temperature plasma ionization source 6 and the nickel source 5 is 10mm. The low-temperature plasma ionization source 6 uses a glass tube with an outer diameter of 6 mm and a thickness of 1 mm as the medium, and a stainless steel cylinder with an inner diameter of 6.1 mm, a thickness of 0.1 mm, and a length of 16 mm is used as a high-voltage radio frequency electrode on the outside of the glass tube. A metal cylindrical rod with an outer diameter of 1.58mm and a length of 100mm is used as the ground electrode, and a radio frequency voltage with a frequency of 25KHz and a peak value of 2KV pp is applied between the two electrodes; the discharge gas is He gas, and the flow rate is 0.2-1L/min; You can choose to add dichloromethane, water vapor and other doping gases to He gas to improve the specificity and sensitivity of explosive detection.
于低温等离子体电离源6后端的气路上设置有离子阱质谱分析器7；从热解析进样器1热解析出来的样品分子经镍源5和低温等离子体电离源6电离后流入离子阱质谱分析器7进行分析。An ion trap mass spectrometer 7 is arranged on the gas path at the rear end of the low temperature plasma ionization source 6; the sample molecules thermally decomposed from the thermal analysis injector 1 flow into the ion trap mass spectrometer after being ionized by the nickel source 5 and the low temperature plasma ionization source 6 Analyzer 7 performs analysis.
实施例2Example 2
热解析进样器1通过热不锈钢金属块对样品进行接触加热。The thermal analysis sampler 1 conducts contact heating on the sample through a hot stainless steel metal block.
载气从热解析进样器1的载气入口2流入，载带样品分子从样品气出口3流出；载气为纯净的干燥空气，载气流速为100-500mL/min，可以选择在空气中添加二氯甲烷、O3等掺杂气体，提高爆炸物检测的选择性和特异性。The carrier gas flows in from the carrier gas inlet 2 of the thermal analysis injector 1, and the sample molecules flow out from the sample gas outlet 3; the carrier gas is pure dry air, and the carrier gas flow rate is 100-500mL/min, and can be selected in the air Add dichloromethane, O 3 and other doping gases to improve the selectivity and specificity of explosive detection.
于热解析进样器1的样品气出口3后端的气路上设置有镍源5；镍源5与样品气出口3的距离为15mm。A nickel source 5 is provided on the gas path at the rear end of the sample gas outlet 3 of the thermal analysis injector 1; the distance between the nickel source 5 and the sample gas outlet 3 is 15 mm.
于热解析进样器1的样品气出口3后端的气路上设置有镍源5；镍源5与样品气出口3的距离为15mm。A nickel source 5 is provided on the gas path at the rear end of the sample gas outlet 3 of the thermal analysis injector 1; the distance between the nickel source 5 and the sample gas outlet 3 is 15 mm.
于镍源5后端的气路上设置有低温等离子体电离源6；低温等离子体电离源6与镍源5的距离为10mm。A low-temperature plasma ionization source 6 is arranged on the gas path at the rear end of the nickel source 5; the distance between the low-temperature plasma ionization source 6 and the nickel source 5 is 10mm.
于低温等离子体电离源6后端的气路上设置有离子迁移谱分析器7；从热解析进样器1热解析出来的样品分子经镍源5和低温等离子体电离源6电离后流入离子迁移谱分析器7进行分析。An ion mobility spectrometer analyzer 7 is arranged on the gas path at the rear end of the low temperature plasma ionization source 6; the sample molecules thermally desorbed from the thermal analysis injector 1 are ionized by the nickel source 5 and the low temperature plasma ionization source 6, and then flow into the ion mobility spectrometer Analyzer 7 performs analysis.
Claims (4)
- A kind of 1. organic and inorganic comprehensive analyzer of explosive, it is characterised in that：Including Thermal desorption injector（1）, sampling cloth（4）, nickel source（5）, low temperature plasma ionization source（6）And analyzer（7）, in Thermal desorption injector（1）On be provided with carrier gas inlet（2）And sample gas outlet（3）；Sample cloth（4）It is placed in Thermal desorption injector（1）It is interior, sample cloth（4）On sample after Thermal desorption sample introduction；Carrier gas is from Thermal desorption injector（1）Carrier gas inlet（2）Flow into, carry sample molecule from sample gas outlet（3）Outflow；In Thermal desorption injector（1）Sample gas outlet（3）Nickel source is provided with the gas circuit of rear end（5）；In nickel source（5）In the gas circuit of rear end It is provided with low temperature plasma ionization source（6）；In low temperature plasma ionization source（6）Analyzer is provided with the gas circuit of rear end （7）.
- 2. the comprehensive analyzer of explosive according to claim 1, it is characterised in that：Thermal desorption injector（1）Contact heating is carried out to sample by thermometal block, or it is non-to sample progress by heating lamp Contact heating.
- 3. the comprehensive analyzer of explosive according to claim 1, it is characterised in that：Described carrier gas is gaseous mixture a kind of or that be two kind gas of the air either in nitrogen.
- 4. the comprehensive analyzer of explosive according to claim 1, it is characterised in that：From Thermal desorption injector（1）The sample molecule separated out is pyrolyzed through nickel source（5）With low temperature plasma ionization source（6）Ionization After flow into analyzer（7）Analyzed；Described analyzer（7）For mass spectrometer or ion mobility spectrometry.
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| CN106645770A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | An on-line detector capable of continuous sample injection and application thereof |
| CN109308990A (en) * | 2018-09-25 | 2019-02-05 | 公安部第三研究所 | Sample introduction system for ion mobility spectrometer |
| CN111105980B (en) * | 2018-10-25 | 2021-01-26 | 中国科学院大连化学物理研究所 | Flash thermal analysis-time-delay purging sample introduction method for drug mixture detection |
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