CN102479662B - Vacuum ultraviolet light ionization source used for high-flux gas sample analysis - Google Patents
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Abstract
本发明涉及质谱分析仪器，具体的说是一种用于高通量气体样品分析的真空紫外光电离源，包括电离源腔体和真空紫外光源；于电离源腔体顶部设置有气体入口，气体样品通过气体入口进入到电离源腔体内部；在电离源腔体内部，沿气体样品流动方向依次设置有相互间隔、同轴、平行的离子引出电极、离子漏斗和差分接口极板；真空紫外光源设置于电离源腔体侧壁上，真空紫外光源发出的真空紫外光平行于离子引出电极的极板并穿过极板间相互间隔的区域进入到离子引出极板的通孔区域。本发明的真空紫外光电离源可有效提高整个质谱仪系统的检测灵敏度，在高通量气体样品分析和环境中有机污染物痕量或超痕量检测领域有着广阔的应用前景。
The invention relates to a mass spectrometry instrument, specifically a vacuum ultraviolet photoionization source for high-throughput gas sample analysis, including an ionization source cavity and a vacuum ultraviolet light source; a gas inlet is arranged on the top of the ionization source cavity, and the gas The sample enters the chamber of the ionization source through the gas inlet; inside the chamber of the ionization source, along the flow direction of the gas sample, there are mutually spaced, coaxial and parallel ion extraction electrodes, ion funnels and differential interface plates; the vacuum ultraviolet light source It is arranged on the side wall of the ionization source cavity, and the vacuum ultraviolet light emitted by the vacuum ultraviolet light source is parallel to the pole plates of the ion extraction electrodes and enters the through hole area of the ion extraction pole plates through the space between the pole plates. The vacuum ultraviolet photoionization source of the invention can effectively improve the detection sensitivity of the entire mass spectrometer system, and has broad application prospects in the field of high-throughput gas sample analysis and trace or ultra-trace detection of organic pollutants in the environment.
Description
技术领域 technical field
本发明涉及质谱分析仪器，具体的说是一种用于高通量气体样品分析的真空紫外光电离源。The invention relates to a mass spectrometer analysis instrument, in particular to a vacuum ultraviolet photoionization source for high-throughput gas sample analysis.
背景技术 Background technique
真空紫外光是指波长小于200nm的深紫外光，它能够使电离能低于其光子能量的物质分子发生单光子电离(Single Proton Ionization，SPI)，产生大量的分子离子，而几乎没有碎片离子。将真空紫外光作为质谱的离子源，得到的谱图简单，可以根据物质的分子量信息进行快速定性和定量分析，在过程分析和有机物在线监测等领域得到越来越广泛的应用。侯可勇[中国发明专利：200610011793.2]将真空紫外灯作为飞行时间质谱的离子源，能够快速检测空气中微量的有机污染物成分；郑培超[中国发明专利：200810022557.X]发明了一种多波长的真空紫外光电离源，可同时检测多种无机化合物和有机化合物。Vacuum ultraviolet light refers to deep ultraviolet light with a wavelength of less than 200nm, which can cause single photon ionization (Single Proton Ionization, SPI) of material molecules whose ionization energy is lower than its photon energy, producing a large number of molecular ions with almost no fragment ions. Using vacuum ultraviolet light as the ion source of mass spectrometry, the spectra obtained are simple, and can be used for rapid qualitative and quantitative analysis based on the molecular weight information of the substance. It has been more and more widely used in the fields of process analysis and online monitoring of organic matter. Hou Keyong [Chinese invention patent: 200610011793.2] used vacuum ultraviolet lamp as the ion source of time-of-flight mass spectrometry, which can quickly detect trace organic pollutants in the air; Zheng Peichao [Chinese invention patent: 200810022557.X] invented a multi-wavelength vacuum UV photoionization source, which can detect many kinds of inorganic compounds and organic compounds simultaneously.
将真空紫外光电离源用于有机物的痕量或超痕量检测时，为了获得足够的检测灵敏度，通常需要高通量的气体样品进样。传统的真空紫外光电离源是将单个真空紫外光源发出的真空紫外光聚焦于电离源内部，使待测气体样品穿过真空紫外光照射区域后被电离，产生的离子在直流电场的引导下通过电离源出口小孔进入质量分析器中检测。在这种结构中，一方面，真空紫外光的光照范围较小，同时受到单个真空紫外光源的强度限制，导致SPI的电离效率不高；另一方面，高通量的气体样品进样还会增加电离源内分子与离子之间的碰撞，使离子发散，电离源内的直流电场对离子起不到汇聚作用，因此降低了离子的传输效率。When vacuum ultraviolet photoionization source is used for trace or ultra-trace detection of organic matter, in order to obtain sufficient detection sensitivity, high-throughput gas sample injection is usually required. The traditional vacuum ultraviolet photoionization source focuses the vacuum ultraviolet light emitted by a single vacuum ultraviolet light source inside the ionization source, so that the gas sample to be measured is ionized after passing through the vacuum ultraviolet light irradiation area, and the generated ions pass through under the guidance of a DC electric field. The small hole at the exit of the ionization source enters the mass analyzer for detection. In this structure, on the one hand, the irradiation range of vacuum ultraviolet light is small, and at the same time, it is limited by the intensity of a single vacuum ultraviolet light source, resulting in low ionization efficiency of SPI; on the other hand, high-throughput gas sample injection will also Increase the collision between molecules and ions in the ionization source to make the ions diverge, and the DC electric field in the ionization source cannot converge the ions, thus reducing the ion transmission efficiency.
发明内容 Contents of the invention
本发明的目的在于提供一种用于高通量气体样品分析的真空紫外光电离源。The object of the present invention is to provide a vacuum ultraviolet photoionization source for high-throughput gas sample analysis.
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:
一种用于高通量气体样品分析的真空紫外光电离源，包括电离源腔体和真空紫外光源，于电离源腔体侧壁上设置有气体出口，气体出口通过真空管路与机械真空泵相连；A vacuum ultraviolet photoionization source for high-throughput gas sample analysis, including an ionization source cavity and a vacuum ultraviolet light source, a gas outlet is arranged on the side wall of the ionization source cavity, and the gas outlet is connected to a mechanical vacuum pump through a vacuum pipeline;
于电离源腔体顶部设置有气体入口，气体样品通过气体入口进入到电离源腔体内部；在电离源腔体内部，沿气体样品流动方向依次设置有相互间隔、同轴、平行的离子引出电极、离子漏斗和差分接口极板；A gas inlet is provided on the top of the ionization source cavity, and the gas sample enters the ionization source cavity through the gas inlet; inside the ionization source cavity, along the flow direction of the gas sample, mutually spaced, coaxial and parallel ion extraction electrodes are arranged in sequence , ion funnel and differential interface plate;
离子引出电极为2块或2块以上中心设有通孔的相互间隔、同轴、平行设置的板式结构；真空紫外光源设置于电离源腔体侧壁上，真空紫外光源发出的真空紫外光平行于离子引出电极的极板并穿过极板间相互间隔的区域进入到离子引出极板的通孔区域；The ion extraction electrodes are two or more plates with through-holes in the center, which are mutually spaced, coaxial, and parallel plate structures; the vacuum ultraviolet light source is arranged on the side wall of the ionization source cavity, and the vacuum ultraviolet light emitted by the vacuum ultraviolet light source is parallel On the pole plate of the ion extraction electrode and through the spaced area between the pole plates to enter the through hole area of the ion extraction pole plate;
离子漏斗为2块或2块以上中心设有通孔的相互间隔、同轴、平行设置的板式结构，离子漏斗沿离子引出电极至差分接口极板的方向、极板上的中心通孔直径逐渐缩小，离子漏斗的极板中心通孔形成一漏斗形区域。The ion funnel is a plate structure with two or more through holes in the center, coaxial, and parallel. Narrowing down, the through hole in the center of the ion funnel forms a funnel-shaped region.
于离子引出电极各极片上依次加载电势逐渐变化的电压，在离子引出电极轴线方向形成均匀或非均匀的离子引出电场，真空紫外光电离产生的离子在离子引出电场的作用下被引入到离子漏斗的漏斗形区域。A voltage with a gradually changing potential is sequentially applied to each pole piece of the ion extraction electrode to form a uniform or non-uniform ion extraction electric field in the axis direction of the ion extraction electrode, and the ions generated by vacuum ultraviolet photoionization are introduced into the ion funnel under the action of the ion extraction electric field funnel-shaped area.
所述的真空紫外光源为气体放电灯光源、激光光源或同步辐射光源。The vacuum ultraviolet light source is a gas discharge lamp light source, a laser light source or a synchrotron radiation light source.
于离子漏斗各极板上连接有射频电源，在漏斗形区域轴线方向形成射频电场，离子引出电极中心区域处产生的离子在离子漏斗中冷却、聚焦。A radio frequency power supply is connected to each electrode plate of the ion funnel, and a radio frequency electric field is formed in the axial direction of the funnel-shaped area, and the ions generated at the central area of the ion extraction electrode are cooled and focused in the ion funnel.
于差分接口极板上设置有差分接口小孔，差分接口小孔与质谱仪的质量分析器相连，即离子引出电极中冷却、聚焦后的离子通过差分接口极板上的差分接口小孔直接引入到质量分析器中；There is a differential interface hole on the differential interface plate, and the differential interface hole is connected to the mass analyzer of the mass spectrometer, that is, the cooled and focused ions in the ion extraction electrode are directly introduced through the differential interface hole on the differential interface plate into the mass analyzer;
所述的质量分析器为飞行时间质量分析器、四级杆质量分析器或离子阱质量分析器。The mass analyzer is a time-of-flight mass analyzer, a quadrupole mass analyzer or an ion trap mass analyzer.
所述的真空紫外光源为1个或2个以上，真空紫外光源发出的真空紫外光以离子引出电极的通孔为中心排列，沿离子引出电极的轴线方向或径向方向排布于离子引出电极的四周，多个真空紫外电源发出的真空紫外光充满整个离子引出极板的通孔中心区域。The vacuum ultraviolet light source is one or more than two, and the vacuum ultraviolet light emitted by the vacuum ultraviolet light source is arranged around the through hole of the ion extraction electrode, and is arranged on the ion extraction electrode along the axis direction or radial direction of the ion extraction electrode Around the surrounding area, the vacuum ultraviolet light emitted by multiple vacuum ultraviolet power sources fills the central area of the through hole of the entire ion extraction plate.
本发明提供的真空紫外光电离源，一方面，通过增大真空紫外光的辐射强度并对进入电离源中的高通量气体样品大面积照射的方法，提高待测样品的电离效率，在电离源中产生更多的待测样品离子；另一方面，在电离源中加入离子漏斗，使得电离源中在大的空间范围内产生的待测样品离子能够有效的通过电离源与质量分析器的接口小孔进入质量分析器中进行检测，大大提高离子的传输效率。本发明的真空紫外光电离源，可有效提高整个质谱仪系统的检测灵敏度，在高通量气体样品分析和环境中有机污染物痕量或超痕量检测领域有着广阔的应用前景。The vacuum ultraviolet photoionization source provided by the present invention, on the one hand, improves the ionization efficiency of the sample to be measured by increasing the radiation intensity of the vacuum ultraviolet light and irradiating a large area of the high-flux gas sample entering the ionization source. On the other hand, an ion funnel is added to the ionization source, so that the sample ions to be measured in a large space in the ionization source can effectively pass through the ionization source and the mass analyzer. The interface hole enters the mass analyzer for detection, which greatly improves the ion transmission efficiency. The vacuum ultraviolet photoionization source of the invention can effectively improve the detection sensitivity of the entire mass spectrometer system, and has broad application prospects in the field of high-throughput gas sample analysis and trace or ultra-trace detection of organic pollutants in the environment.
附图说明 Description of drawings
图1为本发明的真空紫外光电离源结构示意图。Fig. 1 is a schematic diagram of the structure of the vacuum ultraviolet photoionization source of the present invention.
具体实施方式 Detailed ways
请参阅图1，为本发明的结构示意图。本发明的真空紫外光电离源，由电离源腔体3和真空紫外光源5构成。Please refer to FIG. 1 , which is a schematic structural diagram of the present invention. The vacuum ultraviolet photoionization source of the present invention is composed of an ionization source cavity 3 and a vacuum
于电离源腔体3侧壁上设置有气体出口，气体出口通过真空管路与机械真空泵11相连；A gas outlet is provided on the side wall of the ionization source cavity 3, and the gas outlet is connected to the
于电离源腔体3顶部设置有气体入口2，气体样品1通过气体入口2进入到电离源腔体3内部；在电离源腔体3内部，沿气体样品1流动方向依次设置有相互间隔、同轴、平行的离子引出电极4、离子漏斗6和差分接口极板8；A gas inlet 2 is arranged on the top of the ionization source cavity 3, and the gas sample 1 enters the inside of the ionization source cavity 3 through the gas inlet 2; Shaft, parallel ion extraction electrode 4, ion funnel 6 and differential interface plate 8;
离子引出电极4为2块或2块以上中心设有通孔的相互间隔、同轴、平行设置的板式结构；真空紫外光源5设置于电离源腔体3侧壁上，真空紫外光源5发出的真空紫外光12平行于离子引出电极4的极板并穿过极板间相互间隔的区域进入到离子引出极板的通孔区域；The ion extracting electrode 4 is a plate structure with two or more through holes in the center, coaxial and parallel; the vacuum
离子漏斗6为2块或2块以上中心设有通孔的相互间隔、同轴、平行设置的板式结构，离子漏斗6沿离子引出电极4至差分接口极板8的方向、极板上的中心通孔直径逐渐缩小，离子漏斗6的极板中心通孔形成一漏斗形区域7。The ion funnel 6 is a plate structure with two or more centers provided with through holes spaced apart from each other, coaxial, and parallel. The ion funnel 6 is along the direction from the ion extraction electrode 4 to the differential interface plate 8, and the center of the plate. The diameter of the through hole gradually decreases, and the center through hole of the electrode plate of the ion funnel 6 forms a funnel-shaped region 7 .
于离子引出电极4各极片上依次加载电势逐渐变化的电压，在离子引出电极4轴线方向形成均匀或非均匀的离子引出电场，真空紫外光电离产生的离子在离子引出电场的作用下被引入到离子漏斗6的漏斗形区域7。A voltage with a gradually changing potential is sequentially applied to each pole piece of the ion extraction electrode 4, and a uniform or non-uniform ion extraction electric field is formed in the axial direction of the ion extraction electrode 4, and ions generated by vacuum ultraviolet photoionization are introduced into the Funnel-shaped region 7 of ion funnel 6 .
所述的真空紫外光源5为气体放电灯光源、激光光源或同步辐射光源。The vacuum
于离子漏斗6各极板上连接有射频电源，在漏斗形区域7轴线方向形成射频电场，离子引出电极4中心区域处产生的离子在离子漏斗中冷却、聚焦。A radio frequency power supply is connected to each electrode plate of the ion funnel 6, and a radio frequency electric field is formed in the axial direction of the funnel-shaped region 7, and the ions generated at the central region of the ion extraction electrode 4 are cooled and focused in the ion funnel.
于差分接口极板8上设置有差分接口小孔9，差分接口小孔9与质谱仪的质量分析器10相连，即离子引出电极4中冷却、聚焦后的离子通过差分接口极板8上的差分接口小孔9直接引入到质量分析器10中；A differential interface aperture 9 is arranged on the differential interface pole plate 8, and the differential interface aperture 9 is connected to the mass analyzer 10 of the mass spectrometer, that is, the cooled and focused ions in the ion extraction electrode 4 pass through the differential interface pole plate 8. The differential interface aperture 9 is directly introduced into the mass analyzer 10;
所述的质量分析器10为飞行时间质量分析器、四级杆质量分析器或离子阱质量分析器。The mass analyzer 10 is a time-of-flight mass analyzer, a quadrupole mass analyzer or an ion trap mass analyzer.
所述的真空紫外光源5为1个或2个以上，真空紫外光源5发出的真空紫外光以离子引出电极4的通孔为中心排列，沿离子引出电极4的轴线方向或径向方向排布于离子引出电极4的四周，多个真空紫外电源5发出的真空紫外光12充满整个离子引出极板4的通孔中心区域。The vacuum
应用时，高通量的气体样品通过电离源腔体3顶部的气体入口2进入到电离源腔体内部，在整个离子引出电极4的通孔中心区域都能够受到真空紫外光的照射，气体样品中电离能低于真空紫外光子能量的待测物质分子发生单光子电离。光电离产生的离子在离子引出电极4轴线方向的离子引出电场的引导下，进入到离子引出电极4下方设置的离子漏斗6中。离子漏斗6内部形成的射频电场将在大的空间范围内产生的发散的离子冷却、聚焦，使离子以较低的平动能通过差分接口小孔9进入到质量分析器10中进行检测，实现高效的离子传输。电离源腔体3内部未被电离的中性气体分子经由机械真空泵11抽出，以减小质量分析器10中真空系统的负载，维持质量分析时的高真空环境。In application, the high-throughput gas sample enters the interior of the ionization source cavity through the gas inlet 2 at the top of the ionization source cavity 3, and the central area of the through hole of the entire ion extraction electrode 4 can be irradiated by vacuum ultraviolet light. The gas sample Single-photon ionization occurs in the molecules of the substance to be measured whose intermediate ionization energy is lower than the vacuum ultraviolet photon energy. The ions generated by photoionization enter the ion funnel 6 arranged below the ion extraction electrode 4 under the guidance of the ion extraction electric field in the axial direction of the ion extraction electrode 4 . The radio frequency electric field formed inside the ion funnel 6 cools and focuses the divergent ions generated in a large space, so that the ions enter the mass analyzer 10 through the differential interface aperture 9 with low translational energy for detection, achieving high efficiency. ion transport. The unionized neutral gas molecules inside the ionization source chamber 3 are pumped out through the
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| CN103854952A (en) * | 2012-11-30 | 2014-06-11 | 中国科学院大连化学物理研究所 | Mass spectrum vacuum ultraviolet ionization source based on optical-window-free gas discharge lamp |
| CN103871828B (en) * | 2012-12-17 | 2016-05-18 | 中国科学院大连化学物理研究所 | A kind of array photoelectricity transmitting ionization source and application thereof |
| CN103972018B (en) * | 2013-02-01 | 2017-02-08 | 中国科学院大连化学物理研究所 | Radio-frequency electric field enhanced single photon and chemical ionization source |
| CN104282525A (en) * | 2013-07-01 | 2015-01-14 | 中国科学院大连化学物理研究所 | Ion focusing transmission lens under atmosphere pressure |
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| CN108091539A (en) * | 2016-11-21 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of ultraviolet light chemical ionization source based on ion funnel |
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| CN114628226B (en) * | 2020-12-11 | 2024-08-27 | 中国科学院大连化学物理研究所 | A composite photoionization source device for molecular beam mass spectrometry |
| CN114999878B (en) * | 2021-03-01 | 2024-10-29 | 中国科学院化学研究所 | Gas-phase ion molecular reaction device and reaction method |
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