CN111243935A - Ion mobility spectrometer of dielectric barrier discharge ionization source - Google Patents

Ion mobility spectrometer of dielectric barrier discharge ionization source Download PDF

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CN111243935A
CN111243935A CN202010113230.4A CN202010113230A CN111243935A CN 111243935 A CN111243935 A CN 111243935A CN 202010113230 A CN202010113230 A CN 202010113230A CN 111243935 A CN111243935 A CN 111243935A
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ionization source
radio frequency
glass tube
ion mobility
dielectric barrier
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张信华
徐康
黄炜
李柏锦
曹文彬
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Changzhou Institute of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/105Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes

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Abstract

The invention relates to an ion mobility spectrometer, in particular to an ion mobility spectrometer of a dielectric barrier discharge ionization source, which has the advantages of reasonable structure, high detection sensitivity, stability and selectivity by taking dielectric barrier discharge as an ionization source device, and comprises an ionization source, a drift tube and a signal acquisition end, wherein the ionization source comprises a cylindrical shell, a glass tube, a radio frequency electrode, a lead, a radio frequency power supply and an accelerating electrode, the drift tube comprises a metal conducting ring and an insulating ring, the metal conducting ring and the insulating ring are alternately connected, the ionization source comprises a cylindrical shell, a radio frequency power supply, an accelerating electrode, a radio frequency electrode, a quartz glass tube and an accelerating electrode, the accelerating electrode is hermetically arranged at the front end of the cylindrical shell, the quartz glass tube is inserted into the cylindrical shell, the two radio frequency electrodes are inserted into the cylindrical shell and are sleeved on the outer wall of the quartz glass tube, the radio-frequency electrode is also connected with a radio-frequency power supply through a lead.

Description

一种介质阻挡放电电离源的离子迁移谱仪An ion mobility spectrometer with a dielectric barrier discharge ionization source

技术领域technical field

本发明涉及一种离子迁移谱仪,具体为一种介质阻挡放电电离源的离子迁移谱仪。The invention relates to an ion mobility spectrometer, in particular to an ion mobility spectrometer of a dielectric barrier discharge ionization source.

背景技术Background technique

离子迁移谱(Ion Mobility Spectrometry,IMS)是20世纪70年代发展起来的一种检测技术,其分离原理是通过气态离子的迁移率来表征各种不同的化学物质,以对各种物质进行分析检测。离子迁移谱仪具有探测灵敏度高、测量响应快、仪器体积小、造价低等优点,目前已广泛应用于化学毒剂、毒品、危险品和大气环境中的挥发性有机污染物的检测。Ion Mobility Spectrometry (IMS) is a detection technology developed in the 1970s. Its separation principle is to characterize various chemical substances by the mobility of gaseous ions to analyze and detect various substances. . Ion mobility spectrometer has the advantages of high detection sensitivity, fast measurement response, small instrument size and low cost. It has been widely used in the detection of chemical poisons, drugs, dangerous goods and volatile organic pollutants in the atmospheric environment.

常规离子迁移谱仪主要包括采样装置、电离源、漂移管、电控部分、气路循环系统、信号采集及数据处理系统等。其中,漂移管主要由离子反应区、离子门、漂移区三部分组成。电离源是离子迁移谱的一个重要组成部分。现有的离子迁移谱仪最常用的电离源主要有Ni63电离源、电晕放电电离源、光离子化(包括VUV灯以及激光)电离源、电喷雾电离源等。Conventional ion mobility spectrometer mainly includes sampling device, ionization source, drift tube, electronic control part, gas circuit circulation system, signal acquisition and data processing system, etc. Among them, the drift tube is mainly composed of three parts: ion reaction zone, ion gate and drift zone. The ionization source is an important part of ion mobility spectroscopy. The most commonly used ionization sources for existing ion mobility spectrometers mainly include Ni63 ionization sources, corona discharge ionization sources, photoionization (including VUV lamps and lasers) ionization sources, and electrospray ionization sources.

基于Ni63的电离源具有离子化率高、稳定性好及检测灵敏度高的优点,但由于Ni63具有放射性,使离子迁移谱仪的应用受到很大的限制;电晕放电和光离子化电离源适于电离气相样品,并且电离样品的种类有一定的限制;电喷雾电离源适于分析液态样品,但样品需要经过复杂的预处理,电离源的装置结构也较为复杂,不适合做现场检测。所以如何设计一个检测灵敏度高且检测稳定的离子迁移谱仪是一直有待解决的技术难题。The ionization source based on Ni63 has the advantages of high ionization rate, good stability and high detection sensitivity, but due to the radioactivity of Ni63, the application of ion mobility spectrometer is greatly limited; corona discharge and photoionization ionization sources are suitable for Gas-phase samples are ionized, and the types of ionized samples are limited; electrospray ionization sources are suitable for analyzing liquid samples, but the samples need to undergo complex pretreatment, and the device structure of the ionization source is also complex, so it is not suitable for on-site testing. Therefore, how to design an ion mobility spectrometer with high detection sensitivity and stable detection is a technical problem to be solved.

发明内容SUMMARY OF THE INVENTION

本发明要解决的技术问题克服现有的缺陷,提供一种介质阻挡放电电离源的离子迁移谱仪,具有构造合理,以介质阻挡放电作为电离源装置,检测灵敏度、稳定性及选择性高的优点。The technical problem to be solved by the present invention overcomes the existing defects, and provides an ion mobility spectrometer with a dielectric barrier discharge ionization source, which has a reasonable structure, uses the dielectric barrier discharge as the ionization source device, and has high detection sensitivity, stability and selectivity. advantage.

为了解决上述技术问题,本发明提供了如下的技术方案:一种介质阻挡放电电离源的离子迁移谱仪,包括电离源、漂移管和信号采集端,所述电离源包括圆柱形壳体、玻璃管、射频电极、导线、射频电源和加速电极,所述漂移管包括金属导电环和绝缘环,所述金属导电环和绝缘环交替连接,所述电离源包括圆柱形壳体、射频电源、加速电极、射频电极、石英玻璃管和加速电极,所述加速电极密封安装在圆柱形壳体的前端,所述石英玻璃管探入圆柱形壳体内,所述射频电极为两个并探入圆柱形壳体内且套在石英玻璃管外壁,所述射频电极还通过导线与射频电源连接,所述石英玻璃管内含工作气体,还包括采样机构,所述采样机构设在圆柱形壳体内。In order to solve the above technical problems, the present invention provides the following technical solution: an ion mobility spectrometer of a dielectric barrier discharge ionization source, comprising an ionization source, a drift tube and a signal collection end, the ionization source includes a cylindrical shell, a glass tube, radio frequency electrode, wire, radio frequency power supply and acceleration electrode, the drift tube includes a metal conductive ring and an insulating ring, the metal conductive ring and the insulating ring are alternately connected, the ionization source includes a cylindrical shell, a radio frequency power supply, an acceleration Electrode, radio frequency electrode, quartz glass tube and accelerating electrode, the accelerating electrode is sealed and installed at the front end of the cylindrical shell, the quartz glass tube penetrates into the cylindrical shell, and the radio frequency electrodes are two and protrude into the cylindrical shell The casing is sleeved on the outer wall of the quartz glass tube, the radio frequency electrode is also connected to the radio frequency power supply through a wire, the quartz glass tube contains working gas, and also includes a sampling mechanism, and the sampling mechanism is arranged in the cylindrical casing.

作为优选,所述漂移管的前端设有排气口,所述漂移管的尾端设有漂移气入口,所述漂移管的尾端还设有信号采集端。Preferably, the front end of the drift tube is provided with an exhaust port, the rear end of the drift tube is provided with a drift gas inlet, and the rear end of the drift tube is further provided with a signal collection end.

作为优选,所述采样机构为取样管。Preferably, the sampling mechanism is a sampling tube.

作为优选,所述采样机构为样品采样台。Preferably, the sampling mechanism is a sample sampling table.

作为优选,两个射频电极之间的距离为2~3cm,下部的射频电极与石英玻璃管的底端的距离小于5mm。Preferably, the distance between the two RF electrodes is 2-3 cm, and the distance between the lower RF electrode and the bottom end of the quartz glass tube is less than 5 mm.

作为优选,所述玻璃管为石英玻璃管或陶瓷材质的管。Preferably, the glass tube is a quartz glass tube or a ceramic tube.

作为优选,所述玻璃管的内径为1~2mm,壁厚为0.5~2mm。。Preferably, the inner diameter of the glass tube is 1-2 mm, and the wall thickness is 0.5-2 mm. .

本发明有益效果:本发明的介质阻挡放电电离源的离子迁移谱仪作为电离源,介质阻挡放电电离源具有体积小、电能消耗少、放电稳定等优点,在常温常压下可以对气体样品进行电离,产生大量稳定、高能离子。不仅可以避免使用放射性电离源,而且可以直接电离气体、液体或固体样品。同时可以进一步提高离子迁移谱技术的灵敏度、稳定性及选择性,拓宽离子迁移谱的应用领域。Beneficial effects of the present invention: The ion mobility spectrometer of the dielectric barrier discharge ionization source of the present invention is used as an ionization source, and the dielectric barrier discharge ionization source has the advantages of small size, low power consumption, stable discharge, etc. Ionization, producing a large number of stable, high-energy ions. Not only can radioactive ionization sources be avoided, but gaseous, liquid or solid samples can be ionized directly. At the same time, the sensitivity, stability and selectivity of the ion mobility spectrometry technique can be further improved, and the application field of ion mobility spectrometry can be broadened.

附图说明Description of drawings

附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。The accompanying drawings are used to provide a further understanding of the present invention, and constitute a part of the specification, and are used to explain the present invention together with the embodiments of the present invention, and do not constitute a limitation to the present invention.

图1是本发明的介质阻挡放电电离源的离子迁移谱仪的结构示意图。FIG. 1 is a schematic structural diagram of the ion mobility spectrometer of the dielectric barrier discharge ionization source of the present invention.

图2是本发明的介质阻挡放电电离源的离子迁移谱仪的另一种结构示意图。FIG. 2 is another structural schematic diagram of the ion mobility spectrometer of the dielectric barrier discharge ionization source of the present invention.

图中标号:1、导线;2、射频电源;3、玻璃管;4、射频电极;5、圆柱形壳体;6、排气口;7、绝缘环;8、导电环;9、离子门;10、漂移气入口;11、信号采集端;12、加速电极;13、采样机构;14、离子反应区;15、漂移区;16、漂移管。Labels in the figure: 1, wire; 2, radio frequency power supply; 3, glass tube; 4, radio frequency electrode; 5, cylindrical shell; 6, exhaust port; 7, insulating ring; 8, conductive ring; 9, ion gate 10. Drift gas inlet; 11. Signal acquisition end; 12. Accelerating electrode; 13. Sampling mechanism; 14. Ion reaction zone; 15. Drift zone; 16. Drift tube.

具体实施方式Detailed ways

以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, but not to limit the present invention.

在具体实施时,图1和2中所示,一种介质阻挡放电电离源的离子迁移谱仪,所述漂移管16是由若干个金属导电环8和绝缘环7交替排列组成的空腔管,包括离子反应区14、离子门9、漂移区15三部分。所述采样装置安装在电离源中,电离源与漂移管的前端紧密连接,漂移管后端与信号采集端11相接;载气和漂移气在漂移管内部形成气路循环;信号采集端对仪器的信号采集部分进行控制,本发明所涉及离子迁移谱仪的漂移管、载气和漂移气气路循环、电控信号采集及数据处理属于现有技术,不再详述。In the specific implementation, as shown in FIGS. 1 and 2, an ion mobility spectrometer with a dielectric barrier discharge ionization source, the drift tube 16 is a hollow tube composed of several metal conductive rings 8 and insulating rings 7 alternately arranged. , including ion reaction zone 14, ion gate 9, drift zone 15 three parts. The sampling device is installed in the ionization source, the ionization source is closely connected with the front end of the drift tube, and the rear end of the drift tube is connected with the signal acquisition end 11; the carrier gas and the drift gas form a gas circuit circulation inside the drift tube; The signal acquisition part of the instrument is controlled. The drift tube, carrier gas and drift gas gas circuit circulation, electronic control signal acquisition and data processing of the ion mobility spectrometer involved in the present invention belong to the prior art and will not be described in detail.

本发明的特点是:电离源包括圆柱形壳体5、射频电源2、加速电极12、射频电极4和玻璃管3,圆形的加速电极12密封安装在圆柱形壳体5前端,采样机构13从侧壁伸入到圆柱形壳体5内;如图1所示,采样机构13为采样管,如图2所示,采样机构13为采样台,两个射频电极4套在玻璃管3外侧,射频电极4与射频电源2之间通过导线1连接,玻璃管3为石英玻璃管或陶瓷玻璃管,其内径在1~2mm之间,壁厚在0.5~2mm之间,管内导入有工作气体。The characteristics of the present invention are: the ionization source includes a cylindrical shell 5, a radio frequency power supply 2, an accelerating electrode 12, a radio frequency electrode 4 and a glass tube 3, the circular accelerating electrode 12 is sealed and installed at the front end of the cylindrical shell 5, and the sampling mechanism 13 It extends into the cylindrical shell 5 from the side wall; as shown in FIG. 1 , the sampling mechanism 13 is a sampling tube, and as shown in FIG. , the radio frequency electrode 4 and the radio frequency power supply 2 are connected by the wire 1, the glass tube 3 is a quartz glass tube or a ceramic glass tube, its inner diameter is between 1 and 2 mm, and its wall thickness is between 0.5 and 2 mm, and a working gas is introduced into the tube. .

射频电极4为圆环型,两个射频电极4之间的距离为2~3cm,且下部的射频电极4与玻璃管3的底端的距离小于5mm。The radio frequency electrode 4 is annular, the distance between the two radio frequency electrodes 4 is 2-3 cm, and the distance between the lower radio frequency electrode 4 and the bottom end of the glass tube 3 is less than 5 mm.

图1所示的介质阻挡放电电离源离子迁移谱仪,用于直接测试气体样品。采样机构13采用采样管并安装在电离源的圆柱形壳体5的腔体侧壁上,采样管从侧壁伸入到圆柱形壳体内。使用时,玻璃管3内部通入稳定流速的工作气体,接通电源后,工作气体通过介质阻挡放电作用在玻璃管3内部及末端附近产生稳定的等离子体,等离子体在大气压条件下进一步产生反应物离子,待测样品通过采样管导入电离源的圆柱形壳体5内,反应物离子与待测样品发生分子离子反应,产生待测样品产物离子。产物离子在加速电极12助推作用下进入离子反应区,在电场的作用下,产物离子通过周期性开启的离子门9进入漂移区,在环状的导电环8及绝缘环7形成的均匀电场下,产物离子一方面从电场获得能量作定向漂移,另一方面与逆向流动的中性漂移气体分子不断碰撞而损失能量,由于这些产物离子的质量、所带电荷、碰撞截面和空间构型各不相同,故在电场中各自迁移速率不同,使得不同的离子到达信号采集部分的时间不同而得到分离。The dielectric barrier discharge ionization source ion mobility spectrometer shown in Figure 1 is used to directly test gas samples. The sampling mechanism 13 adopts a sampling tube and is installed on the side wall of the cavity of the cylindrical casing 5 of the ionization source, and the sampling tube extends into the cylindrical casing from the side wall. When in use, a working gas with a stable flow rate is introduced into the glass tube 3. After the power is turned on, the working gas generates stable plasma inside and near the end of the glass tube 3 through dielectric barrier discharge, and the plasma further reacts under atmospheric pressure conditions. The sample to be tested is introduced into the cylindrical shell 5 of the ionization source through the sampling tube, and the reactant ions react with the sample to be tested by molecular ions to generate the product ions of the sample to be tested. The product ions enter the ion reaction zone under the boost of the accelerating electrode 12. Under the action of the electric field, the product ions enter the drift zone through the periodically opened ion gate 9, and the uniform electric field formed by the annular conductive ring 8 and the insulating ring 7 On the one hand, the product ions obtain energy from the electric field for directional drift, and on the other hand, they continuously collide with the neutral drift gas molecules in the opposite flow and lose energy. They are not the same, so their migration rates are different in the electric field, so that different ions arrive at the signal acquisition part at different times and are separated.

图2所示的介质阻挡放电电离源离子迁移谱仪,用于直接测试固体或液体样品。采样机构设计为样品采样台,用于承载固体或液体样品。使用时,待测样品通过采样台置入电离源装置内,被电离源电离生成产物离子,产物离子通过加速电极的助推作用进入离子反应区,在电场的作用下,产物离子通过周期性开启的离子门进入漂移区,并在绝缘环及导电环形成的均匀电场下最终到达信号采集及数据处理部分。由于这些产物离子的质量、所带电荷、碰撞截面和空间构型各不相同,故在电场中各自迁移速率不同,使得不同的离子到达信号采集部分的时间不同而得到分离。The dielectric barrier discharge ionization source ion mobility spectrometer shown in Figure 2 is used to directly test solid or liquid samples. The sampling mechanism is designed as a sample sampling stage for carrying solid or liquid samples. When in use, the sample to be tested is placed into the ionization source device through the sampling stage, and is ionized by the ionization source to generate product ions. The product ions enter the ion reaction zone through the boosting action of the accelerating electrode. The ion gate enters the drift region, and finally reaches the signal acquisition and data processing part under the uniform electric field formed by the insulating ring and the conductive ring. Due to the different mass, charge, collision cross-section and spatial configuration of these product ions, their respective migration rates in the electric field are different, so that different ions arrive at the signal acquisition part at different times and are separated.

以上为本发明较佳的实施方式,本发明所属领域的技术人员还能够对上述实施方式进行变更和修改,因此,本发明并不局限于上述的具体实施方式,凡是本领域技术人员在本发明的基础上所作的任何显而易见的改进、替换或变型均属于本发明的保护范围。The above are preferred embodiments of the present invention. Those skilled in the art can also make changes and modifications to the above-mentioned embodiments. Therefore, the present invention is not limited to the above-mentioned specific embodiments. Any obvious improvement, substitution or modification made on the basis of the invention belongs to the protection scope of the present invention.

Claims (7)

1. An ion mobility spectrometer of a dielectric barrier discharge ionization source, characterized in that: the ionization source comprises a cylindrical shell (5), a glass tube (3), a radio frequency electrode (4), a lead (1), a radio frequency power supply (2) and an accelerating electrode (12), wherein the ionization source comprises an ionization source, a drift tube (16) and a signal acquisition end (11), the drift tube (16) comprises a metal conducting ring (8) and an insulating ring (7), the metal conducting ring (8) and the insulating ring (7) are alternately connected, the ionization source comprises the cylindrical shell (5), the radio frequency power supply (2), the accelerating electrode (12), the radio frequency electrode (4), a quartz glass tube (3) and the accelerating electrode (12), the accelerating electrode (12) is hermetically arranged at the front end of the cylindrical shell (5), the quartz glass tube (3) is inserted into the cylindrical shell (5), the radio frequency electrodes (4) are two and are inserted into the cylindrical shell (5) and are sleeved on the outer wall of the quartz glass tube (3), the radio frequency electrode (4) is connected with a radio frequency power supply (2) through a wire (1), the quartz glass tube (3) contains working gas and further comprises a sampling mechanism (13), and the sampling mechanism (13) is arranged in the cylindrical shell (5).
2. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the front end of drift tube (16) is equipped with gas vent (6), the tail end of drift tube (16) is equipped with drift gas entry (10), the tail end of drift tube (16) still is equipped with signal acquisition end (11).
3. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the sampling mechanism (13) is a sampling tube.
4. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the sampling mechanism (13) is a sample sampling platform.
5. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the distance between the two radio frequency electrodes (4) is 2-3 cm, and the distance between the radio frequency electrode (4) at the lower part and the bottom end of the quartz glass tube (3) is less than 5 mm.
6. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the glass tube (3) is a quartz glass tube or a ceramic tube.
7. The ion mobility spectrometer of the dielectric barrier discharge ionization source of claim 1, characterized in that: the inner diameter of the glass tube (3) is 1-2 mm, and the wall thickness is 0.5-2 mm.
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN114609232A (en) * 2020-12-09 2022-06-10 布鲁克光谱有限及两合公司 Ion mobility spectrometer and method for operating an ion mobility spectrometer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114609232A (en) * 2020-12-09 2022-06-10 布鲁克光谱有限及两合公司 Ion mobility spectrometer and method for operating an ion mobility spectrometer
CN114609232B (en) * 2020-12-09 2023-09-19 布鲁克光谱有限及两合公司 Ion mobility spectrometer and method for operating an ion mobility spectrometer

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