CN104282525A - Ion focusing transmission lens under atmosphere pressure - Google Patents
Ion focusing transmission lens under atmosphere pressure Download PDFInfo
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 31
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- 238000004949 mass spectrometry Methods 0.000 claims description 14
- 230000005684 electric field Effects 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 6
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- 238000005040 ion trap Methods 0.000 claims description 2
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- 238000000375 direct analysis in real time Methods 0.000 description 3
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- 238000000688 desorption electrospray ionisation Methods 0.000 description 2
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Abstract
本发明涉及质谱分析仪，具体地说是一种大气压下的离子聚焦传输透镜。包括不锈钢电极环、绝缘介质环以及不锈钢外筒；不锈钢外筒为密闭的筒状结构，左右两端分别设置有离子入口和离子出口；不锈钢电极环和绝缘介质环均为环状结构，分别为2个或3个以上，且相互间隔、同轴、平行设置于靠近离子入口一端的不锈钢外筒内部；不锈钢电极环与不锈钢外筒之间设置有绝缘介质层；离子入口、不锈钢电极环和离子出口相互平行、同轴设置；本发明结构紧凑，使用方便，能够有效的将离子在大气压下聚焦，增强质谱分析仪的灵敏度和测量精确度。
The invention relates to a mass spectrometer, in particular to an ion focusing transmission lens under atmospheric pressure. Including stainless steel electrode ring, insulating medium ring and stainless steel outer cylinder; the stainless steel outer cylinder is a closed cylindrical structure, and the left and right ends are respectively provided with ion inlet and ion outlet; the stainless steel electrode ring and insulating medium ring are ring structures, respectively 2 or more than 3, and spaced from each other, coaxial, and parallel to the inside of the stainless steel outer cylinder near the end of the ion inlet; an insulating medium layer is provided between the stainless steel electrode ring and the stainless steel outer cylinder; the ion inlet, stainless steel electrode ring and ion The outlets are arranged parallel to each other and coaxially; the invention has a compact structure, is convenient to use, can effectively focus ions under atmospheric pressure, and enhance the sensitivity and measurement accuracy of the mass spectrometer.
Description
技术领域technical field
本发明涉及质谱分析仪器，具体地说是一种大气压下的离子聚焦传输透镜，本离子聚焦传输透镜结构紧凑，使用方便，能够有效的将离子在大气压下聚焦传输，增强质谱仪的灵敏度和测量精确度。The invention relates to a mass spectrometer analysis instrument, in particular to an ion focus transmission lens under atmospheric pressure. The ion focus transmission lens has a compact structure, is easy to use, can effectively focus and transmit ions under atmospheric pressure, and enhances the sensitivity and measurement of the mass spectrometer. Accuracy.
背景技术Background technique
原位、无损、现场、快速的分析是在线监测质谱分析技术的发展趋势，在无需样品前处理的条件下对复杂样品直接离子化，可以大大提高质谱分析的效率，加快在线分析的速度。常压离子化技术泛指无需样品预处理，在大气压下对样品进行直接电离，进而快速分析检测的新兴质谱技术。2004年Cooks等提出的电喷雾解析电离（DESI）技术和2005年Cody等提出的实时直接分析（DART）电离技术，大大促进了常压离子化技术的发展。在接下来的几年内，由于分析速度快，检验灵敏度高等优点，这一技术得到蓬勃发展，先后又涌现出近30种常压离子化源。In-situ, non-destructive, on-site, and rapid analysis is the development trend of on-line monitoring mass spectrometry technology. Direct ionization of complex samples without sample pretreatment can greatly improve the efficiency of mass spectrometry and speed up on-line analysis. Atmospheric pressure ionization technology generally refers to the emerging mass spectrometry technology that directly ionizes samples under atmospheric pressure without sample pretreatment, and then quickly analyzes and detects them. The electrospray analytical ionization (DESI) technology proposed by Cooks et al. in 2004 and the direct analysis in real time (DART) ionization technology proposed by Cody et al. in 2005 have greatly promoted the development of atmospheric pressure ionization technology. In the next few years, due to the advantages of fast analysis speed and high detection sensitivity, this technology has been vigorously developed, and nearly 30 kinds of atmospheric pressure ionization sources have emerged successively.
但是，无论是DESI还是DART，几乎所有现存的常压离子化技术，都存在离子收集效率低，难以精确定量分析等缺点。常压离子化源之所以有这些弊端，很大一部分原因要归结于大气压下环境气体较为复杂，由常压离子化源产生的离子，与背景气体发生强烈的碰撞，难以实现有效聚焦。这使得产生的待测物离子，只有很少一部分能够进入到质谱仪当中。不仅如此，进入到质谱仪中的离子不仅复杂，而且较为分散。这给接下来的分析检测过程带来了较大的困难。这也是困扰常压离子化源更加广泛应用的一个重要因素。如果仅仅依靠电场作用，离子聚焦的效果并不理想。However, whether it is DESI or DART, almost all existing atmospheric pressure ionization technologies have disadvantages such as low ion collection efficiency and difficulty in accurate quantitative analysis. A large part of the reason why the atmospheric pressure ionization source has these disadvantages is due to the complexity of the ambient gas under atmospheric pressure. The ions generated by the atmospheric pressure ionization source collide strongly with the background gas, making it difficult to achieve effective focusing. This allows only a small fraction of the analyte ions produced to enter the mass spectrometer. Not only that, but the ions that enter the mass spectrometer are not only complex, but also relatively dispersed. This brings greater difficulties to the subsequent analysis and detection process. This is also an important factor that hinders the wider application of atmospheric pressure ionization sources. If only relying on the electric field, the effect of ion focusing is not ideal.
据此，本发明中利用气流的辅助传输，通过增加抽气泵，在整个离子聚焦传输透镜中形成层流，从而将由解析产生的待测物的气相离子载带进离子聚焦传输透镜中，并与传输透镜中轴向汇聚的电场相结合，使气相离子产生聚焦效果，更为有效的传输至质量分析器，减少离子在传输过程中的损失。Accordingly, in the present invention, the auxiliary transmission of the air flow is used, and a laminar flow is formed in the entire ion focus transmission lens by adding an air pump, so that the gas-phase ions of the analyte generated by analysis are carried into the ion focus transmission lens, and are combined with the ion focus transmission lens. The combination of the axially converged electric field in the transmission lens makes the gas phase ions produce a focusing effect, which is more effectively transmitted to the mass analyzer and reduces the loss of ions during transmission.
发明内容Contents of the invention
本发明的目的在于提供一种用于质谱分析的大气压下的离子聚焦传输透镜，使得由常压离子化源电离产生的离子，在通过此离子聚焦传输透镜后得到有效的汇聚，从而在之后的质谱分析检测中，增强质量分析器的灵敏度和测量精确度。The object of the present invention is to provide an ion focusing transmission lens under atmospheric pressure for mass spectrometry, so that the ions generated by the ionization of the normal pressure ionization source can be effectively converged after passing through the ion focusing transmission lens, so that the subsequent In mass spectrometry detection, the sensitivity and measurement accuracy of the mass analyzer are enhanced.
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:
一种大气压下的离子聚焦传输透镜，包括不锈钢电极环，绝缘介质环和不锈钢外筒，其特征在于：An ion focusing transmission lens under atmospheric pressure, including a stainless steel electrode ring, an insulating medium ring and a stainless steel outer cylinder, is characterized in that:
不锈钢外筒为密闭的筒状结构，于不锈钢外筒左右两个端面上分别设置有离子入口和离子出口；The stainless steel outer cylinder is a closed cylindrical structure, and the ion inlet and ion outlet are respectively set on the left and right end faces of the stainless steel outer cylinder;
不锈钢电极环和绝缘介质环均为环状结构，分别为2个或3个以上；Both the stainless steel electrode ring and the insulating medium ring are ring-shaped, with 2 or more than 3 rings respectively;
不锈钢电极环和绝缘介质环相互间隔、同轴、平行设置于靠近离子入口一端的不锈钢外筒内部；The stainless steel electrode ring and the insulating medium ring are spaced apart from each other, coaxial and parallel, and are arranged inside the stainless steel outer cylinder near the ion entrance;
离子入口、不锈钢电极环和离子出口相互平行、同轴设置；The ion inlet, stainless steel electrode ring and ion outlet are parallel and coaxially arranged;
于靠近离子出口处的不锈钢外筒的侧壁上设置有气体出口；A gas outlet is provided on the side wall of the stainless steel outer cylinder near the ion outlet;
气体出口通过管路与抽气泵连接。The gas outlet is connected with an air pump through a pipeline.
气体出口通过真空管路与一侧抽阀门相连，于侧抽阀门的另一端通过真空管路连接有抽气泵。The gas outlet is connected to the side pumping valve through a vacuum pipeline, and an air pump is connected to the other end of the side pumping valve through a vacuum pipeline.
所述的侧抽阀门为可调节流量的真空阀门，为真空挡板阀、真空蝶阀或者真空针阀。The side pumping valve is a flow-adjustable vacuum valve, such as a vacuum flapper valve, a vacuum butterfly valve or a vacuum needle valve.
一质谱进样管穿过离子出口伸入到不锈钢外筒内部，质谱进样管的入口设置于不锈钢电极环的中心轴线处；A mass spectrometry sampling tube extends into the stainless steel outer cylinder through the ion outlet, and the inlet of the mass spectrometry sampling tube is set at the central axis of the stainless steel electrode ring;
于不锈钢外筒外部、离子入口前端设置有样品承载平台和大气压电离源，产生的气相离子经不锈钢电极环和绝缘介质环的中心区域传输至质谱进样管的入口，进入质量分析器中检测。A sample carrying platform and an atmospheric pressure ionization source are set outside the stainless steel outer cylinder and at the front end of the ion inlet. The gas phase ions generated are transmitted to the inlet of the mass spectrometer sampling tube through the central area of the stainless steel electrode ring and the insulating medium ring, and then enter the mass analyzer for detection.
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、离子阱质量分析器或者离子回旋共振质量分析器；The mass analyzer is a time-of-flight mass analyzer, a quadrupole mass analyzer, an ion trap mass analyzer or an ion cyclotron resonance mass analyzer;
绝缘介质环的内径大于不锈钢电极环的内径。The inner diameter of the insulating medium ring is larger than that of the stainless steel electrode ring.
于各片不锈钢电极环上依次加载不同幅值的电压，在沿离子入口至离子出口的轴线方向上，相邻不锈钢电极环间的电压逐渐递增，且相邻不锈钢电极环之间电压差的递增比例为1:1～1:100，形成场强逐渐增强的电场。Voltages of different amplitudes are sequentially loaded on each stainless steel electrode ring, and the voltage between adjacent stainless steel electrode rings gradually increases along the axis direction from the ion inlet to the ion outlet, and the voltage difference between adjacent stainless steel electrode rings increases gradually. The ratio is 1:1 to 1:100, forming an electric field whose field strength gradually increases.
不锈钢电极环与不锈钢外筒之间设置有绝缘介质层。An insulating medium layer is arranged between the stainless steel electrode ring and the stainless steel outer cylinder.
本发明提供的离子聚焦传输透镜，通过调节电极环形成的电场和抽气泵形成的层流，进而实现对于气相离子的聚焦。具体地说，层流气体将解析产生的待测物的气相离子载带进离子聚焦传输透镜中，并引导气相离子向质量分析器的方向运动。而加载在电极环上的电压，作用于通过离子聚焦透镜的气相离子，使其向轴线汇聚，从而最大限度的减少了气相离子由于发散带来的损失，使更多的气相离子可以进入到质量分析器中，从而提高了质量分析器的灵敏度和测量精确度。The ion focusing transmission lens provided by the present invention realizes focusing on gas phase ions by adjusting the electric field formed by the electrode ring and the laminar flow formed by the air pump. Specifically, the laminar gas carries the gas-phase ions of the analyte produced by the analysis into the ion focusing transmission lens, and guides the gas-phase ions to move toward the mass analyzer. The voltage loaded on the electrode ring acts on the gas phase ions passing through the ion focusing lens to make them converge toward the axis, thereby minimizing the loss of gas phase ions due to divergence and allowing more gas phase ions to enter the mass In the analyzer, the sensitivity and measurement accuracy of the mass analyzer are improved.
附图说明Description of drawings
图1为本发明的离子聚焦传输透镜装置的结构示意图。FIG. 1 is a schematic structural view of the ion focusing transmission lens device of the present invention.
图2为相邻不锈钢电极环电压差比例为1:1时的电场和离子传输轨迹模拟图。Figure 2 is a simulation diagram of the electric field and ion transport trajectory when the voltage difference ratio of adjacent stainless steel electrode rings is 1:1.
图3为相邻不锈钢电极环电压差比例为1:3时的电场和离子传输轨迹模拟图。Figure 3 is a simulation diagram of the electric field and ion transport trajectory when the voltage difference ratio of adjacent stainless steel electrode rings is 1:3.
具体实施方式Detailed ways
请参阅图1，为本发明的结构示意图，图中3为质量分析器，6为气相离子，10为样品承载平台，11为大气压电离源，12为待测样品。本发明的离子聚焦传输透镜，由绝缘介质环1、不锈钢金属外筒2、不锈钢电极环9构成。Please refer to Fig. 1, which is a structural schematic diagram of the present invention, among which 3 is a mass analyzer, 6 is a gas phase ion, 10 is a sample carrying platform, 11 is an atmospheric pressure ionization source, and 12 is a sample to be tested. The ion focusing transmission lens of the present invention is composed of an insulating dielectric ring 1 , a stainless steel metal outer cylinder 2 and a stainless steel electrode ring 9 .
不锈钢外筒2为密闭的筒状结构，于不锈钢外筒2左右两个端面上分别设置有离子入口13和离子出口4；The stainless steel outer cylinder 2 is a closed cylindrical structure, and the ion inlet 13 and the ion outlet 4 are respectively arranged on the left and right end surfaces of the stainless steel outer cylinder 2;
不锈钢电极环9和绝缘介质环1均为环状结构，分别为2个或3个以上；The stainless steel electrode ring 9 and the insulating medium ring 1 are ring-shaped structures, respectively 2 or more than 3;
不锈钢电极环9和绝缘介质环1相互间隔、同轴、平行设置于靠近离子入口13一端的不锈钢外筒2内部；The stainless steel electrode ring 9 and the insulating medium ring 1 are spaced from each other, coaxial and parallel, and are arranged inside the stainless steel outer cylinder 2 near the end of the ion entrance 13;
离子入口13、不锈钢电极环9和离子出口4相互平行、同轴设置，且不锈钢电极环9与不锈钢外筒2之间设置有绝缘介质；The ion inlet 13, the stainless steel electrode ring 9 and the ion outlet 4 are arranged parallel to each other and coaxially, and an insulating medium is arranged between the stainless steel electrode ring 9 and the stainless steel outer cylinder 2;
于靠近离子出口4处的不锈钢外筒2的侧壁上设置有气体出口；A gas outlet is provided on the side wall of the stainless steel outer cylinder 2 near the ion outlet 4;
气体出口通过真空管路与一侧抽阀门8相连，于侧抽阀门8的另一端通过真空管路连接有抽气泵7。通过调节侧抽阀门8，控制抽气泵7的抽速，从而在整个离子聚焦传输透镜系统内形成适当的层流，将由解析产生的待测物的气相离子6载带进离子聚焦系统中，辅助气相离子6的传输，引导气相离子6到达质量分析器3，从而减少气相离子6在传输过程中的损失。The gas outlet is connected to the side pumping valve 8 through a vacuum pipeline, and the other end of the side pumping valve 8 is connected to an air pump 7 through a vacuum pipeline. By adjusting the side pumping valve 8, the pumping speed of the pumping pump 7 is controlled, so that a proper laminar flow is formed in the entire ion focusing transmission lens system, and the gas-phase ions 6 of the analyte produced by analysis are carried into the ion focusing system to assist The transmission of the gas-phase ions 6 guides the gas-phase ions 6 to the mass analyzer 3 , thereby reducing the loss of the gas-phase ions 6 during transmission.
一质谱进样管5穿过离子出口4伸入到不锈钢外筒2内部，质谱进样管5的入口设置于不锈钢电极环9的中心轴线处；A mass spectrometry sampling tube 5 extends into the stainless steel outer cylinder 2 through the ion outlet 4, and the inlet of the mass spectrometry sampling tube 5 is arranged at the central axis of the stainless steel electrode ring 9;
于不锈钢外筒2外部、离子入口13前端设置有样品承载平台10和大气压电离源11，电离源11产生的大量负载有能量和电荷的微小液滴，喷射到样品承载平台10表面的样品12上，快速运动的微小液滴对样品12表面的待测物产生解析作用，并伴随电荷的转移生成待测物的气相离子6。产生的气相离子6经不锈钢电极环9和绝缘介质环1的中心区域传输至质谱进样管5的入口，进入质量分析器3中检测。A sample carrying platform 10 and an atmospheric pressure ionization source 11 are arranged outside the stainless steel outer cylinder 2 and at the front end of the ion inlet 13. A large number of tiny liquid droplets loaded with energy and charge generated by the ionization source 11 are sprayed onto the sample 12 on the surface of the sample carrying platform 10 , the fast-moving micro-droplets generate analytical action on the analyte on the surface of the sample 12, and generate gas-phase ions 6 of the analyte along with the charge transfer. The generated gas phase ions 6 are transmitted to the entrance of the mass spectrometry sampling tube 5 through the central area of the stainless steel electrode ring 9 and the insulating medium ring 1, and then enter the mass analyzer 3 for detection.
绝缘介质环1的厚度为2-5mm，不锈钢电极环9的厚度为10-15mm，且绝缘介质环1的内径大于不锈钢电极环9的内径。The thickness of the insulating medium ring 1 is 2-5mm, the thickness of the stainless steel electrode ring 9 is 10-15mm, and the inner diameter of the insulating medium ring 1 is larger than the inner diameter of the stainless steel electrode ring 9 .
于各片不锈钢电极环9上依次加载不同幅值的电压，在沿离子入口13至离子出口4的轴线方向上，相邻不锈钢电极环9间的电压逐渐递增，且相邻不锈钢电极环9之间电压差的递增比例为1:1～1:100，形成场强逐渐增强的电场。生成的电场使气相离子6随层流进入离子聚焦传输透镜后，沿其轴线方向汇聚，从而减少了由于发散造成的气相离子的损失。Voltages of different amplitudes are sequentially loaded on each piece of stainless steel electrode ring 9. In the axial direction from ion inlet 13 to ion outlet 4, the voltage between adjacent stainless steel electrode rings 9 gradually increases, and the voltage between adjacent stainless steel electrode rings 9 The increasing ratio of the voltage difference between them is 1:1 to 1:100, forming an electric field with gradually increasing field strength. The generated electric field makes the gas-phase ions 6 enter the ion focusing transmission lens with the laminar flow, and then converge along the direction of its axis, thereby reducing the loss of the gas-phase ions due to divergence.
图2和图3为质核比m/z=100的离子，在本发明所述的离子聚焦传输透镜中运动的SIMION软件模拟图。如图所示，9为不锈钢电极环，本模拟实验中，共设置了9块不锈钢电极环；5为质谱的进样管。图中，沿X轴方向的曲线为离子在传输透镜中的运动轨迹，沿Y轴方向的曲线为不锈钢电极环加载电压后形成的电场线。Figure 2 and Figure 3 are SIMION software simulation diagrams of ions with a mass-to-nucleus ratio of m/z=100 moving in the ion focusing transmission lens of the present invention. As shown in the figure, 9 is a stainless steel electrode ring. In this simulation experiment, a total of 9 stainless steel electrode rings are set; 5 is a sample tube for mass spectrometry. In the figure, the curve along the X-axis direction is the trajectory of ions in the transmission lens, and the curve along the Y-axis direction is the electric field line formed after the stainless steel electrode ring is loaded with voltage.
在图2中，相邻不锈钢电极环间的电压差，按照1:1的比例递增，从而在整个离子聚焦传输透镜系统内，形成了比较均匀的电场，在这种电场的作用下，离子随层流气体一起，沿X轴方向运动，汇聚效果较差；而在图3中，相邻不锈钢电极环间的电压差，按照1:3的比例递增，在整个离子聚焦传输透镜系统内，形成了场强逐渐增强的电场，使汇聚效果得到大大改善。In Fig. 2, the voltage difference between the adjacent stainless steel electrode rings is increasing according to the ratio of 1:1, so that a relatively uniform electric field is formed in the entire ion focusing transmission lens system. Under the action of this electric field, the ions follow the The laminar gas moves along the X-axis direction together, and the convergence effect is poor; while in Figure 3, the voltage difference between adjacent stainless steel electrode rings increases according to the ratio of 1:3, and in the entire ion focusing transmission lens system, a The electric field whose field strength gradually increases, greatly improves the convergence effect.
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