CN103745905B - Ion trap mass spectrometer having a particle charge detector to cryogenic - Google Patents

Ion trap mass spectrometer having a particle charge detector to cryogenic Download PDF

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CN103745905B
CN103745905B CN201410005139.5A CN201410005139A CN103745905B CN 103745905 B CN103745905 B CN 103745905B CN 201410005139 A CN201410005139 A CN 201410005139A CN 103745905 B CN103745905 B CN 103745905B
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ion trap
trap mass
liquid nitrogen
provided
nitrogen
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CN103745905A (en
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聂宗秀
占铃鹏
熊彩侨
张宁
刘保湘
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中国科学院化学研究所
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Abstract

本发明公开了一种具有低温电荷检测器的颗粒离子阱质谱仪。 The present invention discloses a particulate ion trap mass spectrometer having a low charge detector. 包括离子阱质量分析器、激光诱导声波解吸电离源和电荷检测器;上端电极和下端电极的轴向上均设有通孔a;环电极的中心位置处设有通孔b;电荷检测器设于离子阱质量分析器的下部,且离子阱质量分析器与电荷检测器之间设有绝缘陶瓷环;电荷检测器表面设有电磁屏蔽罩,电磁屏蔽罩与通孔a的位置相应处设有通孔c;激光诱导声波解吸电离源包括样品靶和激光器;它还包括液氮冷却装置,液氮冷却装置包括密闭腔体,密闭腔体与液氮流入管和液氮流出管相连通;密闭腔体设于电荷检测器的下部,且为接触配合。 An ion trap mass analyzer comprises a laser-induced acoustic desorption ionization detector and a charge source; axially upper electrode and the lower electrode are provided with a through hole a; ring electrodes at the center position of a through-hole B; charge detector provided in the lower part of the ion trap mass analyzer, an insulating ceramic ring is provided between the ion trap mass analyzer and the charge detector; charge detector surface is provided with an electromagnetic shield, the electromagnetic shield through hole provided at a corresponding position C through hole; laser-induced acoustic desorption ionization source comprises a laser and a target sample; further comprising a liquid nitrogen cooling means, the cooling means comprises liquid nitrogen closed cavity, the sealed cavity and nitrogen inlet tube, and nitrogen through the outflow pipe is connected; closed the cavity provided at the lower portion of the charge detector, and is in contact with. 本发明由于采用了液氮流速控制装置,可以对电荷检测器的温度进行调节,从而实现电荷检测器噪音水平的灵活控制。 Since the present invention uses a liquid nitrogen flow rate control means, the temperature can be adjusted to the charge detector, enabling flexible control of the charge detector noise levels.

Description

一种具有低温电荷检测器的颗粒离子阱质谱仪 Ion trap mass spectrometer having a particle charge detector to cryogenic

技术领域 FIELD

[0001] 本发明涉及一种质谱仪,具体涉及一种具有低温电荷检测器的颗粒离子阱质谱仪。 [0001] The present invention relates to a mass spectrometer, an ion trap mass spectrometer particularly relates to particles having a low charge detector.

背景技术 Background technique

[0002] 颗粒物质例如大气溶胶、生物颗粒(病毒、细胞)等广泛存在于自然界中。 [0002] Large aerosol particulate matter e.g., biological particles (virus, cells) and the like are widely found in nature. 由于这些颗粒对于大气环境和人体健康有着重要的影响,因此对其测定和表征是分析测试中的一个重要课题。 Since these particles have an important impact on the atmospheric environment and human health, and therefore the measurement is an important topic to characterize the test analysis. 众所周知,分子的质量是分子固有的性质,同样,颗粒的质量也是表征颗粒物质的一个重要参数。 It is well known that the molecular mass of the molecular properties inherent, similarly, the mass of particles is also an important parameter characterizing particulate matter. 离子阱颗粒质谱是最近发展起来的一种测定颗粒质量的新方法。 Particulate ion trap mass spectrometer is a new method for measuring the mass of particles recently developed. 在实验过程中,由激光诱导声波解吸源解吸出的颗粒物质进入离子阱质量分析器,其质荷比和带电量分别由离子阱质量分析器和电荷检测器测得,从而实现了颗粒质量的快速、准确测定。 During the experiment, a laser-induced acoustic desorption source desorbed particulate matter into the ion trap mass analyzer, and a mass to charge ratio that are obtained with a charge of an ion trap mass analyzer and the measured charge detector, enabling the mass of particles rapid and accurate determination. 以颗粒离子阱质谱为工具,人们已成功测定了聚苯乙烯球及多种细胞的质量。 In ion trap particles as a tool, it has been successfully determined by mass and more cells of polystyrene spheres. 但是,颗粒离子阱质谱还有诸多不足,其中亟待解决的问题之一即为如何降低电荷检测器的背景噪音,提高颗粒质谱的分辨率。 However, particulate ion trap mass spectrometer there are many shortcomings, one of which is the problem to be solved how to reduce background noise charge detector, improving the particle mass resolution. 目前,电荷检测器的平均噪音约为600e,根据颗粒的带电量与颗粒尺寸存在的一定线性关系,只有1 ym以上带电量较高的颗粒才能被有效地检测,这就极大地限制了颗粒离子阱质谱仪对微米级以下较小颗粒的分析。 Currently, the average noise charge detector of about 600E, a linear relationship exists according to a certain charge amount and particle size of the particles, only a higher power than 1 ym particles can be effectively detected band, which greatly limits the ion particles analysis trap mass spectrometer of smaller sub-micron particles.

[0003] 因此,需要提供一种能降低背景噪音的颗粒离子阱质谱仪,以提高质谱仪的检测性能。 [0003] Accordingly, it is necessary to reduce the background noise to provide a particulate ion trap mass spectrometer, the mass spectrometer in order to improve the detection performance.

发明内容 SUMMARY

[0004] 本发明的目的是提供一种具有低温电荷检测器的颗粒离子阱质谱仪,本发明通过对电荷检测器的低温冷却实现其背景噪音的降低,从而为拓展颗粒离子阱质谱的质量范围,实现单个病毒、细菌的质量测定奠定基础。 [0004] The object of the present invention is to provide an ion trap mass spectrometer having a particle charge detector of the low-temperature, low-temperature cooling of the present invention by the charge detector is implemented which reduces the background noise, so as to expand the particles using the ion trap mass achieve a single virus, bacteria lay the foundation for quality measurement.

[0005] 本发明所提供的一种具有低温电荷检测器的颗粒离子阱质谱仪,包括离子阱质量分析器、激光诱导声波解吸电离源和电荷检测器;所述离子阱质量分析器包括上端电极、环电极和下端电极;所述上端电极和所述下端电极分别设于所述环电极的两端,且所述环电极与所述上端电极和所述下端电极之间均设有绝缘陶瓷环;所述上端电极和所述下端电极的轴向上均设有通孔a ;所述环电极的中心位置处设有通孔b ; [0005] The present invention provides a particulate ion trap mass spectrometer having a low charge detector, comprising an ion trap mass analyzer, laser-induced acoustic desorption ionization detector and a charge source; said ion trap mass analyzer includes an upper electrode , the ring electrode and the lower electrode; said upper electrode and said lower electrode are respectively disposed at both ends of said ring electrode, an insulating ceramic ring are provided between the ring electrode and the upper electrode and the lower electrode ; the axial direction of the upper end of the upper electrode and lower electrode are provided with a through hole a; central position of the ring electrode is provided with a through hole B;

[0006] 所述电荷检测器设于所述离子阱质量分析器的下部,且所述离子阱质量分析器与所述电荷检测器之间设有绝缘陶瓷环;所述电荷检测器表面设有一电磁屏蔽罩,所述电磁屏蔽罩与所述通孔a的位置相应处设有通孔c ;所述激光诱导声波解吸电离源包括样品靶和激光器,所述样品靶设于近所述通孔b处; [0006] The charge detector provided at a lower portion of the ion trap mass analyzer, and said ceramic insulating ring is provided between the ion trap mass analyzer and the charge detector; the surface is provided with a charge detector an electromagnetic shield, the electromagnetic shield cover and the through hole at a position corresponding to a through hole C; a laser-induced acoustic desorption ionization source comprises a laser and a target sample, the target sample is provided near the through hole at b;

[0007] 所述颗粒离子阱质谱仪还包括液氮冷却装置,所述液氮冷却装置包括一密闭腔体,所述密闭腔体与液氮流入管和液氮流出管相连通;所述密闭腔体设于所述电荷检测器的下部,且为接触配合。 [0007] The ion trap mass spectrometer further comprises a particulate liquid nitrogen cooling means, said cooling means comprises liquid nitrogen a closed chamber, said closed chamber with liquid nitrogen and liquid nitrogen inflow tube communicating outflow pipe; the closed the cavity provided at the lower portion of the charge detector, and is in contact with.

[0008] 所述的颗粒离子阱质谱仪中,所述密闭腔体的形状和尺寸分别与所述电荷检测器的形状和尺寸相一致,以保证所述液氮冷却装置与所述电荷检测器能够紧密接触。 [0008] The particles in the ion trap mass spectrometer, the closed shape and size of the cavity are consistent with the shape and size of the charge detector to ensure that the liquid nitrogen cooling means and the charge detector It can be in close contact.

[0009] 所述的颗粒离子阱质谱仪中,所述液氮流入管与所述密闭腔体的底部相连通; [0009] The particles in the ion trap mass spectrometer, a nitrogen inlet tube and the closed bottom of the cavity in communication;

[0010] 所述液氮流出管与所述密闭腔体的底部相连通,且延伸至所述密闭腔体的顶部处。 [0010] The bottom liquid nitrogen flowing tube and the closed cavity communicating, and extending to the top of the closed cavity.

[0011] 所述的颗粒离子阱质谱仪中,所述密闭腔体的顶部设有一凹槽,所述液氮流出管延伸至所述凹槽内,这样设置后可使液氮流入后能充满整个封闭腔体,当液氮流速大的时候可以液氮的形式从所述液氮流出管流出,当液氮流速小的时候可以气化的氮气形式从所述液氮流出管流出,从而实现对冷却温度的控制。 [0011] The particles in the ion trap mass spectrometer, the top of the closed chamber is provided with a recess, said nitrogen outflow pipe extending into said recess, so that the liquid nitrogen flows can make settings filled the entire closed chamber, when the large flow rate of liquid nitrogen flowing out of the outflow pipe when liquid nitrogen can form from the liquid nitrogen, liquid nitrogen when a small outflow pipe flows when the flow rate of nitrogen can form from the liquid nitrogen vaporized in order to achieve control of the cooling temperature.

[0012] 所述的颗粒离子阱质谱仪中,所述密闭腔体的高度可为10〜20mm; [0012] The particles in the ion trap mass spectrometer, the closed height of the cavity can be 10~20mm;

[0013] 所述凹槽的高度可为3〜5mm,所述液氮流出管的液氮入口端与所述凹槽顶部之间的距离可为1〜2mm。 [0013] The height of the groove may be 3~5mm, nitrogen inlet end of the outflow pipe with liquid nitrogen distance between the top of the groove may be 1~2mm.

[0014] 所述的颗粒离子阱质谱仪中,所述颗粒离子阱质谱仪还包括液氮流速控制装置;所述液氮流速控制装置包括液氮罐、流量计和微流阀;所述液氮流入管与所述液氮罐相连通,所述液氮罐还与一氮气管路相连通,所述氮气管路上依次设有所述流量计和所述微流阀,且所述流量计设于近所述液氮罐的一端;通过所述氮气管路通入的氮气可使所述液氮罐中的压强增大,从而能将所述液氮罐中的液氮压入到所述密闭腔体中,并可通过通入氮气流速的大小控制液氮流入所述密闭腔体的速度,以实现对所述电荷检测器的温度控制,如需温度恒定时,则可将氮气流速控制为一恒定值;如需升温时,则可提高氮气流速;如需降温时,则可停止通氮气或者降低氮气流速。 [0014] The particulate ion trap mass spectrometer, the ion trap mass spectrometer further comprises a particulate nitrogen flow rate control means; the nitrogen flow rate control means comprises a nitrogen tank, a flow meter and a microfluidic valve; said liquid a nitrogen inlet tube communicating with said tank of liquid nitrogen, a liquid nitrogen tank conduit further communicating with a nitrogen, said nitrogen sequentially with said pipeline and said microfluidic valve flow meter and the flow meter disposed near an end of said tank of liquid nitrogen; pressure within the liquid nitrogen tank is increased by the nitrogen into nitrogen gas enable line, so the liquid nitrogen tank capable of being pressed into liquid nitrogen said sealed cavity, the speed of the liquid nitrogen flows into the closed chamber and is controlled by the flow rate of nitrogen into the size of, for temperature control of the charge detector, when the temperature for constant, the nitrogen flow rate can be It is controlled to a constant value; For when heated, the nitrogen flow rate can be increased; For cooling time, nitrogen may be stopped or reduced nitrogen flow rate.

[0015] 所述的颗粒离子阱质谱仪中,所述电荷检测器底部设有一温度传感器,以实时监测所述电荷检测器的温度。 [0015] The particulate ion trap mass spectrometer, the bottom of the charge detector is provided with a temperature sensor to monitor in real time the temperature of the charge detector.

[0016] 本发明由于采取以上技术方案,其具有以下优点: [0016] As a result of the present invention, the above technical solution, which has the following advantages:

[0017] 1、本发明由于采用液氮对电荷检测器进行降温,最低可使检测器的温度达到-190°C,有效地降低了电荷检测器的热噪音,为将离子阱颗粒质谱的应用范围拓展到细菌及病毒的质量测定奠定了基础。 [0017] 1, the present invention adopts the liquid nitrogen to cool the charge detector, the detector can be the lowest temperature reaches -190 ° C, effectively reducing the thermal noise of the charge detector, particles of the ion trap mass spectrometry applications expand the scope to determine the quality bacteria and viruses basis.

[0018] 2、本发明由于采用了液氮流速控制装置,可以对电荷检测器的温度进行调节,从而实现电荷检测器噪音水平的灵活控制。 [0018] 2, the present invention adopts a liquid nitrogen flow rate control means, the temperature can be adjusted to the charge detector, enabling flexible control of the charge detector noise levels.

[0019] 3、本发明由于采用离子阱质量分析器及电荷检测器,能同时获得颗粒离子的质荷比和电荷数,因此,实现了对颗粒质量及质量分布的快速测定。 [0019] 3, the present invention adopts an ion trap mass analyzer and a charge detector, mass to charge ratio can be obtained simultaneously and the charge number of the ion particles, therefore, to achieve a rapid determination of the mass and the mass distribution of particles.

[0020] 4、本发明由于采用离子阱质量分析器,其对真空度的要求低,能够在更加粗略的真空条件下工作,所需的真空条件只需要机械栗就可以提供,为颗粒质谱仪的进一步简化提供了有利的条件。 [0020] 4, the present invention adopts an ion trap mass analyzer, which requires a low degree of vacuum, it is possible to work in a more rough vacuum conditions, the desired vacuum condition can only provide a mechanical Li, a particle mass spectrometer further simplified to provide favorable conditions.

附图说明 BRIEF DESCRIPTION

[0021]图1是本发明具有低温电荷检测器的颗粒离子阱质谱仪的结构示意图。 [0021] FIG. 1 is a schematic structural diagram of an ion trap of the present invention, particles having a low charge detector of the mass spectrometer.

[0022] 图2是本发明具有低温电荷检测器的颗粒离子阱质谱仪的剖视图。 [0022] FIG. 2 is a sectional view of the ion trap particles of the present invention having a low charge detector of the mass spectrometer.

[0023] 图3是本发明颗粒质谱仪中激光诱导声波解吸电离源的示意图。 [0023] FIG. 3 is a schematic view of a laser-induced acoustic desorption ionization mass spectrometer of the present invention particles.

[0024]图4是本发明颗粒质谱仪中液氮流速控制装置的结构示意图。 [0024] FIG. 4 is a structural diagram of a mass spectrometer according to the present invention, the particle flow rate control means of liquid nitrogen.

[0025] 图5是本发明颗粒质谱仪在不同温度条件下电荷检测器的噪音。 [0025] FIG. 5 of the present invention is a particle mass spectrometer under different temperature conditions noise charge detector.

[0026] 图中各标记如下: [0026] FIG each labeled as follows:

[0027] 1上端电极、2环电极、3下端电极、4电荷检测器、5陶瓷环、6信号输出端、7模拟信号输入端、8液氮冷却装置、9密闭腔体、10液氮流入管、11液氮流出管、12凹槽、13激光诱导声波解吸电离源、14样品靶、15激光、16流量计、17氮气管路、18液氮罐、19微流阀。 [0027] One end of the electrode, the ring electrode 2, the lower end of the electrode 3, charge detector 4, a ceramic ring 5, a signal output terminal 6, the analog signal input terminal 7, a liquid nitrogen cooling unit 8, the closed chamber 9, flows into the liquid nitrogen 10 tube, nitrogen outlet tube 11, grooves 12, 13 of the laser-induced acoustic desorption ionization source, the target sample 14, laser 15, flow meter 16, a nitrogen gas conduit 17, nitrogen tank 18, a micro valve 19.

具体实施方式 Detailed ways

[0028] 下述结合附图对本发明做进一步说明,但本发明并不局限于以下实施例。 [0028] The following in conjunction with the accompanying drawings of the present invention will be further described, but the present invention is not limited to the following embodiments.

[0029] 如图1和图2所示,本发明提供的具有低温电荷检测器的颗粒离子阱质谱仪包括激光诱导声波解吸电离源13、离子阱质量分析器、电荷检测器4、液氮冷却装置8以及液氮流速控制装置。 [0029] FIGS. 1 and 2, the present invention provides particles having a low charge ion trap mass spectrometer detector comprises a laser-induced acoustic desorption ionization source 13, an ion trap mass analyzer, charge detector 4, liquid nitrogen cooling means 8 and liquid nitrogen flow rate control means. 该离子阱质量分析器包括一个上端电极1、环电极2和下端电极3,上端电极1、环电极2和下端电极3均为双曲面形,且其外周围均为长方形。 The ion trap mass analyzer comprising an upper electrode 1, electrode 2 and the lower ring electrode 3, an upper electrode, lower electrode 2 and the ring electrode 3 are double curved shape, and the outer periphery are rectangular. 环电极2的半径为10mm,上端电极1和下端电极3与阱中心之间的距离均为7.07mm,上端电极1和下端电极3与环电极2之间均设有绝缘陶瓷环(图中未示),避免其相互接触发生短路。 Radius of the ring electrode 2 of 10mm, the distance between the upper electrode 1 and the lower electrode 3 and the center of the well are 7.07mm, an upper electrode 1 and the lower electrode 3 and the ring electrode has an insulating ceramic ring (not between 2 shown), which prevent a short circuit contact with each other. 上端电极1和下端电极3的轴向上均设有通孔a(图中未示),环电极2的中心位置处设有通孔b。 The axial end of the electrode 1 and the lower electrode are provided with through holes 3 a (not shown), at a central position of ring 2 is provided with a through hole electrode b. 电荷检测器4设于离子阱质量分析器的下部,两者距离为10mm,且两者之间以绝缘陶瓷环5隔开。 Charge detector 4 provided in the lower portion of the ion trap mass analyzer, both the distance of 10mm, and spaced between the insulating ceramic ring 5. 为避免电磁干扰,电荷检测器4表面附加一电磁屏蔽罩(图中未示),且在该电磁屏蔽罩上与通孔a的位置相应处设有通孔c (图中未示)。 In order to avoid electromagnetic interference, an additional charge detector surface 4 a electromagnetic shield (not shown), and a through-hole C (not shown) in the electromagnetic shield cover and the through hole at a corresponding position. 电荷检测器4上包括信号输出端6和模拟信号输入端7。 Charge detector 6 comprises a signal output terminal 7 and the analog signal input terminal 4. 信号输出端6与外部信号采集装置相连,用于采集电荷检测器的信号。 Signal output terminal 6 is connected with an external signal acquisition means for collecting the signal charge detector. 在模拟信号输入端7输入一个标准的模拟信号可实现对电荷检测器响应的校正。 A standard analog input signal at an input terminal 7 can achieve the correction of the analog signal charge detector response.

[0030] 如图3所示,本发明中激光诱导声波解吸电离源13包括样品靶14和激光器(图中未示),样品靶14设于近通孔b处,激光器发射的激光15对样品进行解吸电离。 [0030] 3, according to the present invention, a laser induced acoustic desorption ionization source 13 comprises a target sample and a laser 14 (not shown), the sample b is provided at the target 14 near the through hole, the laser light 15 emitted from the laser sample desorption ionization.

[0031 ] 如图1和图2所示,液氮冷却装置8包括一密闭腔体9,该密闭腔体9与液氮流入管10和液氮流出管11相连通。 [0031] FIGS. 1 and 2, liquid nitrogen cooling device 8 comprises a closed chamber 9, the closed chamber 9 and the liquid nitrogen inflow tube 10 and outflow tube 11 is connected through the nitrogen. 密闭腔体9设于电荷检测器4的下部,且为接触配合。 Closed chamber 9 provided in a lower portion of the charge detector 4, and the mating contact. 液氮流入管10与密闭腔体9的底部相连通;密闭腔体9的顶部设有一凹槽12,液氮流出管11与密闭腔体9的底部相连通,且延伸至凹槽12内,这样能使液氮流入后能充满整个密闭腔体9,在液氮流速大的时候以液氮形式从液氮流出管11流出,液氮流速小的时候以气化的氮气形式从液氮流出管11流出,从而实现对冷却温度的控制。 Nitrogen inlet pipe 10 and the bottom of the closed chamber 9 in communication; top-tight chamber 9 is provided with a recess 12, the liquid nitrogen and the bottom outflow pipe 11 in the closed chamber 9 communicates, and extends into the groove 12, this enables the liquid nitrogen flows can fill the entire cavity 9 closed, liquid nitrogen from the liquid nitrogen in the form of the outflow pipe 11 flows in liquid nitrogen when a large flow rate, the flow rate of liquid nitrogen when a small form of nitrogen flowing out from the liquid nitrogen vaporized the outflow tube 11, thus controlling the cooling temperature.

[0032] 本发明中的液氮流速是通过如图4所示的液氮流速控制装置控制的。 [0032] The liquid nitrogen flow rate of the present invention is achieved by a liquid nitrogen flow rate control device shown in FIG. 4 control. 该液氮流速控制装置包括液氮罐18、流量计16和微流阀19 ;其中液氮流入管7与液氮罐18相连通,液氮罐18还与一氮气管路17相连通,在氮气管路17上依次设置流量计16和微流阀19,且流量计16设于近液氮罐18的一端。 The liquid nitrogen flow rate control means comprises a liquid nitrogen tank 18, flow meter 16, and the micro valve 19; wherein the nitrogen inlet tube 7 communicates with the liquid nitrogen tank 18, the liquid nitrogen tank 18 and further through a nitrogen line 17 are connected, in nitrogen line flow meter 16 are sequentially provided a microfluidic valves 19 and 17, and flow meter 16 provided at one end near the liquid nitrogen tank 18.

[0033] 使用上述液氮流速控制装置控制液氮流速的过程如下:高纯氮气从氮气管路17入口进入,其流速可由流量计16进行实时测量并由微流阀19进行调控。 [0033] Using the above liquid nitrogen flow rate control means controls the flow rate of nitrogen as follows: high purity nitrogen from the conduit 17 into the inlet nitrogen at a flow rate measured by the flow meter 16 in real time by the micro valve 19 to regulate flow. 流入的氮气使液氮罐18中的压强增大,从而将液氮压入到液氮冷却装置的密闭腔体9中。 Blowing nitrogen into the liquid nitrogen tank 18 so that the pressure is increased, liquid nitrogen and thus pressed into the closed cavity of the liquid nitrogen cooling means 9. 温度稳定时氮气的流速可控制在0.4〜0.6mL/min,需要降温时流速可增加氮气流速至0.8〜1.0mL/min,需要升温时则可停止氮气流入或调低氮气流速在0.3mL/min以下。 Nitrogen gas flow rate may be controlled when temperature stabilized at 0.4~0.6mL / min, nitrogen flow required to cool the increased flow 0.8~1.0mL / min, nitrogen gas may be stopped when necessary inflow temperature increase or decrease in nitrogen flow 0.3mL / min the following.

[0034] 为了能够实时监控电荷检测器4的温度,可在电荷检测器4底部设置一温度传感器(图中未示)。 [0034] In order to real-time monitor the temperature of the charge detector 4 can be provided with a temperature sensor (not shown) at the bottom of the charge detector 4.

[0035] 本发明颗粒离子阱质谱仪中,密闭腔体9的高度可为10〜20mm,凹槽12的高度可为3〜5mm,液氮流出管11的液氮入口端与凹槽12顶部之间的距离可为1〜2mm。 [0035] The particulate ion trap mass spectrometer of the present invention, the height of the closed chamber 9 can be 10~20mm, the height of the groove 12 may be 3~5mm, 12 at the top of the liquid nitrogen in liquid nitrogen outflow pipe 11 and the inlet end of the recess the distance between can be 1~2mm.

[0036] 使用本发明具有低温电荷检测器的颗粒离子阱质谱仪时,利用激光诱导声波解吸电离源13使颗粒解吸并进入到离子阱质量分析器中,通过改变离子阱的囚禁条件,即扫描囚禁电压或频率使离子变得不稳定而抛出阱外被电荷检测器所检测。 When using the present invention has a particle charge detector cryogenic ion trap mass spectrometer [0036], using a laser-induced acoustic desorption ionization source 13 and the particles are desorbed into the ion trap mass analyzer, ion trap by changing the trapping conditions, i.e., the scanning voltage or frequency trapped ions to become unstable and thrown out of the wells is detected by the charge detector. 利用液氮冷却装置和液氮流速控制装置可将电荷检测器的温度控制在特定的范围。 The cooling device using liquid nitrogen, and liquid nitrogen flow rate control device may control the temperature of the charge detector is within a specific range.

[0037] 当温度降低时,电荷检测器的噪音明显降低,如图5所示,在常温(20°C)时,检测器的平均噪音为0.01V,如图5a)所示;当温度降低为-64°c时,检测器的平均噪音降低了一半,为0.005V,如图5b)所示。 [0037] When the temperature decreases, the charge detector noise significantly reduced, as shown in FIG. 5, at room temperature (20 ° C), the average noise detector is 0.01V, as shown in FIG 5a) below; when the temperature decreases It is -64 ° c, the average noise detector is reduced by half, to 0.005V, FIG. 5b) shown in FIG.

[0038] 在上述检测过程中,离子阱内气压可控制在1.50〜3.0OPa之间的一固定值,环电极所加RF电压可为800〜1000V之间一固定值,RF频率扫描区间可为450〜100Hz。 [0038] In the detection process, the pressure within the ion trap can be controlled to a fixed value between 1.50~3.0OPa, ring electrodes applied RF voltage may be a fixed value between 800~1000V, RF frequency sweep interval may be 450~100Hz.

[0039] 上述各实施例仅用于说明本发明,电压的施加方式、各部件的结构、尺寸、设置位置及形状都是可以有所变化的,在本发明技术方案的基础上,凡根据本发明原理对个别部件进行的改进和等同变换,均不应排除在本发明的保护范围之外。 [0039] The above-described embodiments are merely illustrative of the invention, the applied voltage mode, structure, size, position and shape of each set are members may vary, based on the aspect of the present invention, where the present the individual components of the inventive principles modifications and equivalents transformation, should not be excluded from the scope of the present invention.

Claims (6)

1.一种具有低温电荷检测器的颗粒离子阱质谱仪,包括离子阱质量分析器、激光诱导声波解吸电离源和电荷检测器;所述离子阱质量分析器包括上端电极、环电极和下端电极;所述上端电极和所述下端电极分别设于所述环电极的两端,且所述环电极与所述上端电极和所述下端电极之间均设有绝缘陶瓷环;所述上端电极和所述下端电极的轴向上均设有通孔a ;所述环电极的中心位置处设有通孔b ; 所述电荷检测器设于所述离子阱质量分析器的下部,且所述离子阱质量分析器与所述电荷检测器之间设有绝缘陶瓷环;所述电荷检测器表面设有一电磁屏蔽罩,所述电磁屏蔽罩与所述通孔a的位置相应处设有通孔c ;所述激光诱导声波解吸电离源包括样品靶和激光器,所述样品靶设于近所述通孔b处;其特征在于: 所述颗粒离子阱质谱仪还包括液氮冷却装置,所述液氮 A charge detector having a cryogenic particle ion trap mass spectrometer, an ion trap mass analyzer comprising a laser-induced acoustic desorption ionization detector and a charge source; said ion trap mass analyzer includes an upper electrode, lower electrode and the ring electrode ; said upper electrode and said lower electrode are respectively disposed at both ends of the ring electrode and has an insulating ceramic ring between the ring electrode and the upper electrode and the lower electrode; and the upper electrode the lower end of the upper electrode has a through hole in the axial direction a; central position of the ring electrode is provided with a through hole B; the charge detector provided at a lower portion of the ion trap mass analyzer, and said ion an insulating ceramic ring is provided between the charge trap mass analyzer and the detector; the charge detector surface is provided with an electromagnetic shield, the electromagnetic shield cover and the through hole at a position corresponding to a through hole c ; a laser-induced acoustic desorption ionization source comprises a laser and a target sample, the target sample is provided near the through hole at b; wherein: said particulate ion trap mass spectrometer further comprises liquid nitrogen cooling means, said liquid nitrogen 冷却装置包括一密闭腔体,所述密闭腔体与液氮流入管和液氮流出管相连通;所述密闭腔体设于所述电荷检测器的下部,且为接触配合; 所述密闭腔体的顶部设有一凹槽,所述液氮流出管延伸至所述凹槽内。 The cooling device comprises a closed chamber, said closed chamber with liquid nitrogen and liquid nitrogen inflow tube communicating outflow pipe; the closed chamber provided in a lower portion of the charge detector, and is in contact with; the closed cavity the top body is provided with a recess, said nitrogen outflow pipe extending into the groove.
2.根据权利要求1所述的颗粒离子阱质谱仪,其特征在于:所述密闭腔体的形状和尺寸分别与所述电荷检测器的形状和尺寸相一致。 2. The granules according to claim ion trap mass spectrometer of claim 1, wherein: the shape and dimensions of the cavity are closed consistent with the shape and size of the charge detector.
3.根据权利要求1所述的颗粒离子阱质谱仪,其特征在于:所述液氮流入管与所述密闭腔体的底部相连通; 所述液氮流出管与所述密闭腔体的底部相连通,且延伸至所述密闭腔体的顶部处。 3. The particle of claim ion trap mass spectrometer of claim 1, wherein: said liquid nitrogen inflow tube and the closed bottom cavity communicating; nitrogen of the bottom outflow pipe to the closed cavity communicating, and extending to the top of the closed cavity.
4.根据权利要求1所述的颗粒离子阱质谱仪,其特征在于:所述密闭腔体的高度为10 〜20mm ; 所述凹槽的高度为3〜5mm,所述液氮流出管的液氮入口端与所述凹槽顶部之间的距离为1〜2_。 Particle according to claim ion trap mass spectrometer of claim 1, wherein: said cavity is tightly closed 10 ~20mm; the height of the groove is 3~5mm, the liquid nitrogen flowing tube distance between the top end and the nitrogen inlet is 1~2_ recess.
5.根据权利要求1所述的颗粒离子阱质谱仪,其特征在于:所述颗粒离子阱质谱仪还包括液氮流速控制装置; 所述液氮流速控制装置包括液氮罐、流量计和微流阀;所述液氮流入管与所述液氮罐相连通,所述液氮罐还与一氮气管路相连通,所述氮气管路上依次设有所述流量计和所述微流阀,且所述流量计设于近所述液氮罐的一端。 5. The granules according to claim ion trap mass spectrometer of claim 1, wherein: said particles further comprising a liquid nitrogen ion trap mass spectrometer flow rate control means; the nitrogen flow rate control means comprises a nitrogen tank, a flow meter and a micro valve; the liquid nitrogen inflow tube communicating with said tank of liquid nitrogen, a liquid nitrogen tank conduit further communicating with a nitrogen, said nitrogen sequentially with said flow meter pipeline and the microfluidic valve and a flow meter is provided near one end of the liquid nitrogen tank.
6.根据权利要求1所述的颗粒离子阱质谱仪,其特征在于:所述电荷检测器底部设有一温度传感器。 The particulate ion trap mass spectrometer according to claim 1, wherein: the bottom of a charge detector provided with a temperature sensor.
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