CN106770071A - The measuring system and method for a kind of free radical - Google Patents
The measuring system and method for a kind of free radical Download PDFInfo
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Abstract
本发明公开一种自由基的测量系统及方法，该系统包括：激光器、样品池、信号收集模块、高速门控探测器、信号处理模块；所述激光器发出的光源路径、气体进入所述进气采样孔的路径与所述高速门控探测器的探测通道彼此相互正交且连通；所述高速门控探测器与光子计数器连接；所述光子计数器用于对门控探测器探测的激发光进行测量；所述激发光为所述激光器发出的光源与所述气体相遇激发出的激发光；所述高速门控探测器基于高效光电倍增管设计，通过高压开关和光电倍增管分压电路调制电压，控制所述高压门控探测器的探测时序。采用本发明的方法及系统能够提高测量大气高活性自由基的测量精度。
The invention discloses a free radical measurement system and method. The system includes: a laser, a sample pool, a signal collection module, a high-speed gating detector, and a signal processing module; the light source path emitted by the laser, and the gas entering the intake air The path of the sampling hole and the detection channel of the high-speed gated detector are mutually orthogonal and communicated; the high-speed gated detector is connected to a photon counter; the photon counter is used to measure the excitation light detected by the gated detector The excitation light is the excitation light excited by the encounter between the light source emitted by the laser and the gas; the high-speed gated detector is designed based on a high-efficiency photomultiplier tube, and the voltage is modulated by a high-voltage switch and a photomultiplier tube voltage divider circuit, Controlling the detection timing of the high voltage gated detector. The method and the system of the invention can improve the measurement accuracy of measuring atmospheric highly active free radicals.
Description
技术领域technical field
本发明涉及大气化学领域，特别是涉及一种自由基的测量系统及方法。The invention relates to the field of atmospheric chemistry, in particular to a free radical measurement system and method.
背景技术Background technique
自由基是地球对流层大气中的重要成分和氧化剂，在对流层光化学过程中起着核心作用。自由基的任何变化趋势是至关重要的，决定了大气中各种重要痕量气体的寿命及浓度分布，影响着不同重要气体的转化并最终促使对流层臭氧或颗粒物产生。大气灰霾问题与活跃的大气自由基化学反应过程可能存在紧密联系。因此准确、实时、动态地探测对流层自由基浓度对研究大气层光化学过程起着重要的作用。Free radicals are important constituents and oxidants in the Earth's tropospheric atmosphere and play a central role in tropospheric photochemical processes. Any change trend of free radicals is crucial, which determines the lifetime and concentration distribution of various important trace gases in the atmosphere, affects the transformation of different important gases, and finally promotes the generation of tropospheric ozone or particulate matter. Atmospheric haze may be closely related to the active chemical reaction process of atmospheric free radicals. Therefore, accurate, real-time and dynamic detection of tropospheric free radical concentration plays an important role in the study of atmospheric photochemical processes.
由于自由基浓度特别低，且非常活跃，其准确监测一直是大气化学领域的一大难题。目前光致发光法是重要的监测手段之一，通过测量光源与气体相遇激发出的激光强度来计算待测物浓度，但发射光强度相对激发光弱数个量极，且寿命非常短(微秒级别以下)。由于发射光的分辨提取是测量的关键，采用传统光学滤光片等方式可以将不同波段的光源及激发出的激光分离出来，但不能应用于光源和激发出的激光同波段的情况，同时也会直接影响对大气高活性自由基的测量精度。Due to the extremely low concentration and high activity of free radicals, their accurate monitoring has always been a major problem in the field of atmospheric chemistry. At present, the photoluminescence method is one of the important monitoring methods. The concentration of the analyte is calculated by measuring the laser intensity excited by the encounter between the light source and the gas. However, the emitted light intensity is several orders of magnitude weaker than the excitation light, and the lifespan is very short (micro below the second level). Since the resolution and extraction of emitted light is the key to measurement, light sources of different bands and excited lasers can be separated by using traditional optical filters, etc. It will directly affect the measurement accuracy of highly active free radicals in the atmosphere.
发明内容Contents of the invention
本发明的目的是提供一种自由基的测量系统及方法，能够解决测量大气高活性自由基手段缺乏、测量精度低的问题。The purpose of the present invention is to provide a measurement system and method for free radicals, which can solve the problems of lack of means for measuring highly active free radicals in the atmosphere and low measurement accuracy.
为实现上述目的，本发明提供了如下方案：To achieve the above object, the present invention provides the following scheme:
一种自由基的测量系统，包括：激光器、样品池、信号收集模块、高速门控探测器、信号处理模块；A measurement system for free radicals, including: a laser, a sample pool, a signal collection module, a high-speed gating detector, and a signal processing module;
所述样品池上方设置有进气采样孔，所述样品池下方经波纹管接真空泵组，所述真空泵组与压力计和控制阀连接；An air intake sampling hole is arranged above the sample pool, and a vacuum pump group is connected to the bottom of the sample pool through a bellows, and the vacuum pump group is connected with a pressure gauge and a control valve;
所述样品池为低压密闭池；The sample pool is a low-pressure airtight pool;
所述信号收集模块安置在所述样品池的一侧；The signal collection module is arranged on one side of the sample pool;
所述激光器发出的光源路径、气体进入所述进气采样孔的路径与所述高速门控探测器的探测通道彼此相互正交且连通；The path of the light source emitted by the laser, the path of gas entering the intake sampling hole, and the detection channel of the high-speed gated detector are mutually orthogonal and communicated;
所述高速门控探测器与光子计数器连接；所述光子计数器用于对所述高速门控探测器探测激发光的脉冲信号进行测量；所述激发光为所述激光器发出的光源与所述气体相遇激发出的激发光；The high-speed gated detector is connected with a photon counter; the photon counter is used to measure the pulse signal of the high-speed gated detector to detect the excitation light; the excitation light is the light source emitted by the laser and the gas The excitation light emitted by the encounter;
所述高速门控探测器通过高压开关和光电倍增管分压电路调制电压，控制所述高压门控探测器的探测时序；The high-speed gated detector modulates the voltage through a high-voltage switch and a photomultiplier tube voltage divider circuit to control the detection timing of the high-voltage gated detector;
所述光子计数器与所述信号处理模块电连接；所述信号处理模块用于计算待测物浓度；The photon counter is electrically connected to the signal processing module; the signal processing module is used to calculate the concentration of the analyte;
所述激发光经所述信号收集模块采集后传入到所述高速门控探测器进行探测，再经前置放大器将信号放大后进入所述光子计数器进行测量，并在所述信号处理模块中进行浓度计算。After the excitation light is collected by the signal collection module, it is transmitted to the high-speed gating detector for detection, and then the signal is amplified by the preamplifier and then enters the photon counter for measurement, and the signal is amplified in the signal processing module Perform concentration calculations.
可选的，所述信号收集模块，具体包括：Optionally, the signal collection module specifically includes:
沿所述信号探测光轴方向上设置有反射镜、透镜组、窄带滤波片的聚焦透镜组；A focusing lens group including a mirror, a lens group, and a narrow-band filter is arranged along the direction of the signal detection optical axis;
所述反射镜与所述聚焦透镜组置于荧光收集位置的两侧，所述反射镜反射的光线也经过所述聚焦透镜组收集；The reflector and the focus lens group are placed on both sides of the fluorescence collection position, and the light reflected by the reflector is also collected by the focus lens group;
所述窄带滤波片用于滤除光源及环境杂散光干扰；The narrow-band filter is used to filter out light source and ambient stray light interference;
所述聚焦透镜组分为透镜前组和透镜后组；The focusing lens group is divided into a lens front group and a lens rear group;
所述透镜前组为科勒照明系统，所述透镜后组为物方远心系统。The lens front group is a Kohler illumination system, and the lens rear group is an object-space telecentric system.
可选的，所述高速门控探测器，具体包括：Optionally, the high-speed gating detector specifically includes:
延时信号发生器、开关电路、高压电源、电阻、电容、光电倍增管；Delayed signal generator, switching circuit, high voltage power supply, resistor, capacitor, photomultiplier tube;
所述延时信号发生器与所述开关电路的控制端相连；The delay signal generator is connected to the control terminal of the switch circuit;
所述高压电源与所述开关电路的输入端相连；The high-voltage power supply is connected to the input end of the switch circuit;
所述电容与所述开关电路的输出端相连；The capacitor is connected to the output end of the switch circuit;
所述电阻串联在所述高压电源和所述电容之间；The resistor is connected in series between the high voltage power supply and the capacitor;
所述光电倍增管的阳极与所述光子计数器相连；The anode of the photomultiplier tube is connected to the photon counter;
所述光电倍增管的阴极与所述高压电源相连；The cathode of the photomultiplier tube is connected to the high voltage power supply;
所述光电倍增管的打拿极并联在所述电阻和所述电容之间。The dynode of the photomultiplier tube is connected in parallel between the resistor and the capacitor.
可选的，所述激光器为高重频可调谐激光器。Optionally, the laser is a high repetition rate tunable laser.
可选的，还包括：Optionally, also include:
参考池，所述参考池安装在所述激光器的旁边，将所述激光器发出的部分激光分束引入参考池中，参考池内放置与样品池成分相近或一致，但浓度更高的激发物，通过探测参考池内高浓度反应物信号强度对激光器输出波长进行监控和反馈调节，维持信号稳定输出；A reference cell, the reference cell is installed next to the laser, and part of the laser split beam emitted by the laser is introduced into the reference cell, and an exciter with a composition similar to or consistent with the sample cell but with a higher concentration is placed in the reference cell. Detect the signal intensity of high-concentration reactants in the reference cell to monitor and feedback the output wavelength of the laser to maintain a stable signal output;
可选的，还包括：Optionally, also include:
光路系统，所述光路系统设置在所述参考池和所述样品池之间；an optical path system, the optical path system is arranged between the reference cell and the sample cell;
所述光路系统用于将所述激发光扩束准直后传输到所述样品池内。The optical path system is used to expand and collimate the excitation light and transmit it into the sample cell.
可选的，还包括：Optionally, also include:
光电二极管，所述光电二极管与所述样品池连接。a photodiode, the photodiode is connected to the sample cell.
一种自由基的测量方法，所述测量方法应用于一种自由基的测量系统，包括：激光器、样品池、信号收集模块、高速门控探测器、信号处理模块；A free radical measurement method, the measurement method is applied to a free radical measurement system, including: a laser, a sample pool, a signal collection module, a high-speed gate detector, a signal processing module;
所述样品池上方设置有进气采样孔，所述样品池下方经波纹管接真空泵组，所述真空泵组与压力计和控制阀连接；An air intake sampling hole is arranged above the sample pool, and a vacuum pump group is connected to the bottom of the sample pool through a bellows, and the vacuum pump group is connected with a pressure gauge and a control valve;
所述样品池为低压密闭池；The sample pool is a low-pressure airtight pool;
所述信号收集模块安置在所述样品池的一侧；The signal collection module is arranged on one side of the sample pool;
所述高速门控探测器安置在所述信号收集模块焦点位置；The high-speed gated detector is placed at the focal point of the signal collection module;
所述激光器发出的光源路径、气体进入所述进气采样孔的路径与所述高速门控探测器的探测通道彼此相互正交且连通；The path of the light source emitted by the laser, the path of gas entering the intake sampling hole, and the detection channel of the high-speed gated detector are mutually orthogonal and communicated;
所述高速门控探测器与光子计数器连接；所述光子计数器用于对所述高速门控探测器探测激发光的脉冲信号进行测量；所述激发光为所述激光器发出的光源与所述气体相遇激发出的激发光；The high-speed gated detector is connected with a photon counter; the photon counter is used to measure the pulse signal of the high-speed gated detector to detect the excitation light; the excitation light is the light source emitted by the laser and the gas The excitation light emitted by the encounter;
所述高速门控探测器通过高压开关和光电倍增管分压电路调制电压，控制所述高压门控探测器的探测时序；The high-speed gated detector modulates the voltage through a high-voltage switch and a photomultiplier tube voltage divider circuit to control the detection timing of the high-voltage gated detector;
所述光子计数器与所述高速门控探测器电连接；The photon counter is electrically connected to the high-speed gated detector;
所述光子计数器与所述信号处理模块电连接；所述信号处理模块用于计算待测物浓度；The photon counter is electrically connected to the signal processing module; the signal processing module is used to calculate the concentration of the analyte;
所述激发光经所述信号收集模块采集后传入到所述高速门控探测器进行探测，再经前置放大器将信号放大后进入所述光子计数器进行测量，并在信号处理模块中进行浓度计算；After the excitation light is collected by the signal collection module, it is transmitted to the high-speed gating detector for detection, and then the signal is amplified by the preamplifier and then enters the photon counter for measurement, and the concentration is measured in the signal processing module. calculate;
所述方法包括：The methods include:
获取激发光源；Obtain an excitation light source;
对所述激发光源进行扩束准直后，与待测物相遇激发出激发光；After the excitation light source is expanded and collimated, it encounters the object to be measured and excites the excitation light;
探测所述激发光的位置光强；detecting the position light intensity of the excitation light;
对所述激发光进行测量，得到第一测量结果；measuring the excitation light to obtain a first measurement result;
根据所述第一测量结果和所述位置光强分析所述待测物浓度。Analyzing the concentration of the analyte according to the first measurement result and the light intensity at the position.
可选的，所述对所述发射光进行甄别测量，得到第一测量结果之前，还包括：Optionally, before the screening measurement of the emitted light is obtained, the first measurement result further includes:
通过调制光电倍增管一个或多个打拿极的加载电压控制高速门控探测器探测所述发射光；controlling the high-speed gate detector to detect the emitted light by modulating the loading voltage of one or more dynodes of the photomultiplier tube;
利用所述光子计数器对所述发射光进行甄别测量。A discriminative measurement of the emitted light is performed using the photon counter.
可选的，所述调制光电倍增管一个或多个打拿极的加载电压，具体包括：Optionally, the modulation of the loading voltage of one or more dynodes of the photomultiplier tube specifically includes:
利用延时信号发生器对光电倍增管的开关电路进行控制，从而调制所述光电倍增管一个或多个打拿极的加载电压。A delay signal generator is used to control the switch circuit of the photomultiplier tube, thereby modulating the loading voltage of one or more dynodes of the photomultiplier tube.
根据本发明提供的具体实施例，本发明公开了以下技术效果：采用本发明中自由基的测量系统及方法，通过进气采样孔完成采集，样品从样品池真空进入，通过真空泵组和压力反馈实现维持样品池内压力稳定，采用自由射流膨胀的方式实现高效低损耗采样，并利用高压调制电路和分压电路对光电倍增管进行高速门控控制，使得高速门控光电倍增管能够高效收集和测量发射光信号，提高了探测灵敏度，提高了对大气中自由基的检测精度，同时，采用光子计数器实现了超低强度激发光信号的光子检测，实现低浓度高活性自由基的精确检测。According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects: the measurement system and method of free radicals in the present invention are adopted, the collection is completed through the intake sampling hole, the sample enters from the sample pool under vacuum, and is passed through the vacuum pump group and pressure feedback The pressure in the sample cell is kept stable, the free jet expansion method is used to achieve high-efficiency and low-loss sampling, and the high-voltage modulation circuit and voltage divider circuit are used to perform high-speed gating control on the photomultiplier tube, so that the high-speed gating photomultiplier tube can be collected and measured efficiently The emission of light signals improves the detection sensitivity and the detection accuracy of free radicals in the atmosphere. At the same time, a photon counter is used to realize the photon detection of ultra-low-intensity excitation light signals, and realize the accurate detection of low-concentration and high-activity free radicals.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the accompanying drawings required in the embodiments. Obviously, the accompanying drawings in the following description are only some of the present invention. Embodiments, for those of ordinary skill in the art, other drawings can also be obtained according to these drawings without paying creative labor.
图1为本发明实施例测量系统结构示意图；Fig. 1 is a schematic structural diagram of a measuring system according to an embodiment of the present invention;
图2为本发明实施例高速门控探测器电路图；Fig. 2 is the circuit diagram of the high-speed gating detector of the embodiment of the present invention;
图3为本发明实施例测量方法流程图。Fig. 3 is a flowchart of a measurement method according to an embodiment of the present invention.
具体实施方式detailed description
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
本发明的目的是提供一种自由基的测量系统及方法，能够解决测量大气高活性自由基手段缺乏、测量精度低的问题。The purpose of the present invention is to provide a measurement system and method for free radicals, which can solve the problems of lack of means for measuring highly active free radicals in the atmosphere and low measurement accuracy.
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图和具体实施方式对本发明作进一步详细的说明。In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
图1为本发明实施例测量系统结构示意图，如图1所示，一种自由基的测量系统，包括：激光器101、样品池102、信号收集模块103、高速门控探测器105、信号处理模块109；Fig. 1 is a schematic structural diagram of the measurement system of an embodiment of the present invention. As shown in Fig. 1, a free radical measurement system includes: a laser 101, a sample pool 102, a signal collection module 103, a high-speed gating detector 105, and a signal processing module 109;
所述样品池102上方设置有进气采样孔106，所述样品池102下方经波纹管接真空泵组107，所述真空泵组107与压力计113和控制阀连接；所述激光器101所发出的光可通过光路转折、光纤传导等方式将激光导入样品池；The top of the sample pool 102 is provided with an intake sampling hole 106, and the bottom of the sample pool 102 is connected to a vacuum pump group 107 through a bellows, and the vacuum pump group 107 is connected with a pressure gauge 113 and a control valve; the light emitted by the laser 101 The laser can be introduced into the sample cell through optical path turning, optical fiber transmission, etc.;
所述样品池102为低压密闭池；The sample cell 102 is a low-pressure airtight cell;
所述信号收集模块103安置在所述样品池102的一侧；The signal collection module 103 is arranged on one side of the sample pool 102;
所述激光器101发出的光源路径、气体进入所述进气采样孔106的路径与所述高速门控探测器105的探测通道彼此相互正交且连通；The path of the light source emitted by the laser 101, the path of gas entering the intake sampling hole 106, and the detection channel of the high-speed gated detector 105 are mutually orthogonal and communicated;
所述高速门控探测器105与光子计数器108连接；所述光子计数器108用于对所述高速门控探测器探测的激发光的脉冲信号进行测量；所述激发光为所述激光器101发出的光源与所述气体相遇激发出的激发光；The high-speed gating detector 105 is connected with a photon counter 108; the photon counter 108 is used to measure the pulse signal of the excitation light detected by the high-speed gating detector; the excitation light is emitted by the laser 101 The excitation light excited by the encounter between the light source and the gas;
所述高速门控探测器105基于门控光电倍增管104设计，通过高压开关1052和光电倍增管104内部分压电路调制电压，控制所述高压门控探测器104的探测时序。The high-speed gated detector 105 is designed based on the gated photomultiplier tube 104 , and the detection timing of the high-voltage gated detector 104 is controlled by modulating the voltage through the high-voltage switch 1052 and the internal voltage divider circuit of the photomultiplier tube 104 .
所述光子计数器108与所述信号处理模块109电连接；The photon counter 108 is electrically connected to the signal processing module 109;
所述信号处理模块109用于计算待测物浓度；The signal processing module 109 is used to calculate the concentration of the analyte;
所述激发光经所述信号收集模块103采集后传入到所述高速门控探测器105进行探测，再经前置放大器将信号放大后进入所述光子计数器108进行测量，并在信号处理模块109中进行浓度计算。After the excitation light is collected by the signal collection module 103, it is transmitted to the high-speed gated detector 105 for detection, and then the signal is amplified by the preamplifier and then enters the photon counter 108 for measurement, and is processed in the signal processing module Concentration calculations are performed in 109.
可选的，所述信号收集模块103，具体包括：Optionally, the signal collection module 103 specifically includes:
沿所述信号探测光轴方向上设置有反射镜、透镜组、窄带滤波片的聚焦透镜组；A focusing lens group including a mirror, a lens group, and a narrow-band filter is arranged along the direction of the signal detection optical axis;
所述反射镜与所述聚焦透镜组置于荧光收集位置的两侧，所述反射镜反射的光线也经过所述聚焦透镜组收集；The reflector and the focus lens group are placed on both sides of the fluorescence collection position, and the light reflected by the reflector is also collected by the focus lens group;
所述窄带滤波片用于滤除光源及环境杂散光干扰；The narrow-band filter is used to filter out light source and ambient stray light interference;
所述聚焦透镜组分为透镜前组和透镜后组；The focusing lens group is divided into a lens front group and a lens rear group;
所述透镜前组为科勒照明系统，所述透镜后组为物方远心系统。The lens front group is a Kohler illumination system, and the lens rear group is an object-space telecentric system.
可选的，图2为本发明实施例高速门控探测器电路图，如图2所示，所述高速门控探测器105，具体包括：Optionally, FIG. 2 is a circuit diagram of a high-speed gating detector according to an embodiment of the present invention. As shown in FIG. 2 , the high-speed gating detector 105 specifically includes:
延时信号发生器1051、开关电路1052、高压电源1053、电阻R、电容C、光电倍增管104；Delay signal generator 1051, switch circuit 1052, high voltage power supply 1053, resistor R, capacitor C, photomultiplier tube 104;
所述延时信号发生器1051与所述开关电路1052的控制端相连；The delay signal generator 1051 is connected to the control terminal of the switch circuit 1052;
所述高压电源1053与所述开关电路1052的输入端相连；The high voltage power supply 1053 is connected to the input end of the switch circuit 1052;
所述电容C与所述开关电路1054的输出端相连；The capacitor C is connected to the output terminal of the switch circuit 1054;
所述电阻R串联在所述高压电源1053和所述电容C之间；The resistor R is connected in series between the high voltage power supply 1053 and the capacitor C;
所述光电倍增管104的阳极1055与所述光子计数器108相连；The anode 1055 of the photomultiplier tube 104 is connected to the photon counter 108;
所述光电倍增管104的阴极1056与所述高压电源1053相连；The cathode 1056 of the photomultiplier tube 104 is connected to the high voltage power supply 1053;
所述光电倍增管104的打拿极1057并联在所述电阻R和所述电容C之间。The dynode 1057 of the photomultiplier tube 104 is connected in parallel between the resistor R and the capacitor C.
可选的，所述激光器101为高重频可调谐激光器。Optionally, the laser 101 is a high repetition rate tunable laser.
可选的，还包括：Optionally, also include:
参考池110，所述参考池110安装在所述激光器101旁边，将主光路的部分激光分束引入参考池，参考池110内放置与样品池102成分相近或一致，但浓度更高的反应物(激发物)，所述激光器发射出的光诱导击穿光谱技术探测参考池内高浓度反应物信号强度对激光器输出波长进行监控和反馈调节，维持信号稳定输出。Reference pool 110, the reference pool 110 is installed next to the laser 101, and part of the laser split beam of the main optical path is introduced into the reference pool, and a reactant with a composition similar to or identical to that of the sample pool 102 but with a higher concentration is placed in the reference pool 110 (exciter), the light-induced breakdown spectroscopy technology emitted by the laser detects the signal intensity of the high-concentration reactant in the reference cell to monitor and feedback the output wavelength of the laser to maintain a stable output of the signal.
可选的，还包括：Optionally, also include:
光路系统111，所述光路系统设置在所述参考池110和所述样品池102之间；An optical path system 111, the optical path system is arranged between the reference pool 110 and the sample pool 102;
所述光路系统111用于将激光扩束准直后传输到样品池内；The optical system 111 is used to collimate the expanded laser beam and transmit it into the sample cell;
所述光路系统包括转折镜、光纤、扩束准直镜等。The optical path system includes turning mirrors, optical fibers, beam expander collimating mirrors and the like.
可选的，还包括：Optionally, also include:
光电二极管112，所述光电二极管112与所述样品池102连接。A photodiode 112 , the photodiode 112 is connected to the sample cell 102 .
采用该系统能够解决测量大气高活性自由基手段缺乏、测量精度低的问题；采用高强度窄带光源照射目标物产生激发光信号，通过环境控制、设置参考池维持光源稳定输出；样品池为低压密闭池，样品从腔体采样真空进入，通过真空泵组和压力反馈实现维持腔体压力稳定，通过自由射流膨胀的方式实现高效低损耗采样；采用光学透镜组完成信号的高效采集，设置窄带滤光片消除杂散光干扰；通过设计的高压调制电路和光电倍增管供电电路实现光电倍增管特定时序内的高速开启和关闭，避免激发光源杂散光损坏探测器或影响其响应，同时达到超短寿命发射光的测量目的。结合光子计数技术实现低强度光子信号的累积测量，进而分析待测物浓度。The use of this system can solve the problems of lack of means for measuring highly active free radicals in the atmosphere and low measurement accuracy; high-intensity narrow-band light sources are used to irradiate the target to generate excitation light signals, and the stable output of the light source is maintained through environmental control and setting of reference cells; the sample cell is low-pressure airtight The sample enters from the cavity sampling vacuum, the cavity pressure is kept stable through the vacuum pump group and pressure feedback, and the high-efficiency and low-loss sampling is realized through free jet expansion; the optical lens group is used to complete the efficient signal collection, and the narrow-band filter is set Eliminate stray light interference; through the designed high-voltage modulation circuit and photomultiplier tube power supply circuit, the photomultiplier tube can be turned on and off at a high speed within a specific time sequence, so as to avoid stray light from the excitation light source from damaging the detector or affecting its response, while achieving ultra-short lifetime emission measurement purpose. Combining photon counting technology to realize the cumulative measurement of low-intensity photon signals, and then analyze the concentration of the analyte.
本发明还包括一种自由基的测量方法，所述测量方法应用于一种自由基的测量系统，包括：激光器101、样品池102、信号收集模块103、高速门控探测器105、信号处理模块109；The present invention also includes a free radical measurement method, which is applied to a free radical measurement system, including: a laser 101, a sample pool 102, a signal collection module 103, a high-speed gate detector 105, and a signal processing module 109;
所述样品池102上方设置有进气采样孔106，所述样品池102下方经波纹管接真空泵组107，所述真空泵组与压力计113和控制阀连接；An air intake sampling hole 106 is arranged above the sample pool 102, and the bottom of the sample pool 102 is connected to a vacuum pump group 107 through a bellows, and the vacuum pump group is connected with a pressure gauge 113 and a control valve;
所述样品池102为低压密闭池；The sample cell 102 is a low-pressure airtight cell;
所述信号收集模块103安置在所述样品池102的一侧；The signal collection module 103 is arranged on one side of the sample pool 102;
所述激光器101发出的光源路径、气体进入所述进气采样孔106的路径与所述高速门控探测器105的探测通道彼此相互正交且连通；The path of the light source emitted by the laser 101, the path of gas entering the intake sampling hole 106, and the detection channel of the high-speed gated detector 105 are mutually orthogonal and communicated;
所述高速门控探测器105与光子计数器108连接；所述光子计数器108用于对探测的激发光进行测量；所述激发光为所述激光器101发出的光源与所述气体相遇激发出的激发光；The high-speed gated detector 105 is connected to a photon counter 108; the photon counter 108 is used to measure the detected excitation light; the excitation light is the excitation generated by the encounter between the light source emitted by the laser 101 and the gas Light;
所述高速门控探测器105基于门控光电倍增管104设计，通过高压开关1052和光电倍增管104内部分压电路调制电压，控制所述高压门控探测器104的探测时序。The high-speed gated detector 105 is designed based on the gated photomultiplier tube 104 , and the detection timing of the high-voltage gated detector 104 is controlled by modulating the voltage through the high-voltage switch 1052 and the internal voltage divider circuit of the photomultiplier tube 104 .
所述光子计数器108与所述高速门控探测器105电连接；The photon counter 108 is electrically connected to the high-speed gating detector 105;
所述光子计数器108与所述信号处理模块109电连接；所述信号处理模块109用于计算待测物浓度；The photon counter 108 is electrically connected to the signal processing module 109; the signal processing module 109 is used to calculate the concentration of the analyte;
所述激发光经所述信号收集模块103采集后传入到所述高速门控探测器105进行探测，再经前置放大器将信号放大后进入所述光子计数器108进行测量，并在所述信号处理模块109中进行浓度计算；图3为本发明实施例测量方法流程图，如图3所示，所述方法包括：After the excitation light is collected by the signal collection module 103, it is transmitted to the high-speed gated detector 105 for detection, and then the signal is amplified by the preamplifier and then enters the photon counter 108 for measurement. Concentration calculation is carried out in the processing module 109; Fig. 3 is a flow chart of the measurement method of the embodiment of the present invention, as shown in Fig. 3, the method includes:
步骤S301：获取激发光源；Step S301: Obtain an excitation light source;
步骤S302：对所述激发光源进行将激光扩束准直后传输到样品池内，与待测物相遇激发出激发光；Step S302: expand and collimate the excitation light source, transmit it into the sample cell, and excite the excitation light when it encounters the object to be tested;
步骤S303：探测所述激发光的位置光强；Step S303: detecting the position light intensity of the excitation light;
步骤S304：对所述激发光进行测量，得到第一测量结果；Step S304: Measure the excitation light to obtain a first measurement result;
步骤S305：根据所述第一测量结果和所述位置光强分析所述待测物浓度。Step S305: Analyze the concentration of the analyte according to the first measurement result and the light intensity at the position.
可选的，所述对所述发射光进行甄别测量，得到第一测量结果之前，还包括：Optionally, before the screening measurement of the emitted light is obtained, the first measurement result further includes:
通过调制光电倍增管一个或多个打拿极1057的加载电压控制高速门控探测器探测所述发射光；controlling the high-speed gated detector to detect the emitted light by modulating the loading voltage of one or more dynodes 1057 of the photomultiplier tube;
利用所述光子计数器对所述发射光进行甄别测量。A discriminative measurement of the emitted light is performed using the photon counter.
可选的，所述调制光电倍增管一个或多个打拿极1057的加载电压，具体包括：Optionally, the modulation of the loading voltage of one or more dynodes 1057 of the photomultiplier tube specifically includes:
利用延时信号发生器对光电倍增管的开关电路进行控制，从而调制所述光电倍增管一个或多个打拿极1057的加载电压。A delay signal generator is used to control the switch circuit of the photomultiplier tube, so as to modulate the loading voltage of one or more dynodes 1057 of the photomultiplier tube.
采用本发明的自由基的测量方法可以实现对基于光致发光法的大气活性自由基的在线监测。在气体低压扩张的情况下，系统可以稳定高速采集大气中待测气体，减少气体碰撞，延长待测物寿命；同时低压条件可减少干扰气体影响，提高发射光寿命。光学系统的设计减少系统的杂散光干扰，高速门控探测器高效收集和测量发射光信号。门控系统通过利用光电倍增管的调制方式实现几十纳秒的所述高速门控探测器开启和响应恢复，短时间内完成测量状态的切换，避免激发光对探测器的响应干扰，实现发射光的时序分辨选择测量。采用光子计数技术精确分别强度超低的概率产生的发射光信号，可实现发射光的高灵敏度累积采集。The free radical measuring method of the invention can realize the online monitoring of the atmospheric active free radical based on the photoluminescence method. In the case of gas expansion at low pressure, the system can stably collect the gas to be measured in the atmosphere at high speed, reduce gas collisions, and prolong the life of the object to be tested; at the same time, low pressure conditions can reduce the influence of interfering gases and increase the life of emitted light. The design of the optical system reduces the stray light interference of the system, and the high-speed gate detector efficiently collects and measures the emitted light signal. The gating system uses the modulation method of the photomultiplier tube to realize the opening and response recovery of the high-speed gating detector in tens of nanoseconds, completes the switching of the measurement state in a short time, avoids the response interference of the excitation light to the detector, and realizes the emission Timing-resolved selective measurements of light. The photon counting technology is used to accurately distinguish the emitted light signals generated by the probability of ultra-low intensity, which can realize the high-sensitivity cumulative collection of emitted light.
为了便于理解，采用如下实施例方式进行描述：For ease of understanding, the following examples are used for description:
激发光源通过环境控制和参考池110的反馈控制维持输出信号稳定，经光路系统111后导入样品池，同时光电二极管112探测激发光的位置光强。所述激光器101发出的光源路径、气体进入所述进气采样孔106的路径与所述高速门控探测器104的探测通道彼此相互正交且连通；气流通过真空泵组107从样品池采样口抽取进入样品池102，压力计113探测和反馈腔内压力，气流扩张膨胀后与激发光束相交产生发射光；发射光经信号收集模块103采集后传入高速门控探测器105，信号放大后经光子计数器108进行甄别测量，并在所述信号处理模块109中进一步处理。延时信号发生器1051实现激发器101、高速门控探测器105、光子计数器108的时序统一。The excitation light source maintains a stable output signal through the environment control and the feedback control of the reference cell 110 , and then enters the sample cell through the optical system 111 , while the photodiode 112 detects the position and light intensity of the excitation light. The path of the light source emitted by the laser 101, the path of gas entering the intake sampling hole 106, and the detection channel of the high-speed gated detector 104 are mutually orthogonal and communicated; the gas flow is drawn from the sampling port of the sample pool by the vacuum pump group 107 After entering the sample cell 102, the pressure gauge 113 detects and feeds back the pressure in the cavity. After the gas flow expands and expands, it intersects with the excitation beam to generate emitted light; the emitted light is collected by the signal collection module 103 and then transmitted to the high-speed gating detector 105. After the signal is amplified, it passes through the photon A counter 108 performs a discrimination measurement and further processes it in said signal processing module 109 . The delay signal generator 1051 realizes the unification of the timing of the exciter 101 , the high-speed gate detector 105 and the photon counter 108 .
所述高速门控探测器105主要包括延时信号发生器1051、开关电路1054、高压电源1053、电阻R、电容C、光电倍增管104等；所述开关电路1054为MOSFET开关电路。高压电源1053提供信号的各路稳定电压输出，延时信号发生器1051控制开关电路1054的调制输出，改变叠加到光电倍增管1052的打拿级1057的电压，以实现与光电倍增管阴极1056及其他打拿级的电势差调制，实现光电倍增管的快速门控。光电倍增管104开启是采集待测信号，由阳极1055输出，经放大后导入光子计数器108进行采集。The high-speed gating detector 105 mainly includes a delay signal generator 1051, a switch circuit 1054, a high voltage power supply 1053, a resistor R, a capacitor C, a photomultiplier tube 104, etc.; the switch circuit 1054 is a MOSFET switch circuit. The high-voltage power supply 1053 provides each stable voltage output of the signal, and the delay signal generator 1051 controls the modulation output of the switch circuit 1054 to change the voltage superimposed on the dynode 1057 of the photomultiplier tube 1052, so as to realize the connection with the photomultiplier tube cathode 1056 and Potential difference modulation of other dynar levels enables fast gating of photomultiplier tubes. The photomultiplier tube 104 is turned on to collect the signal to be measured, which is output by the anode 1055 and then amplified and then introduced into the photon counter 108 for collection.
本发明设计特制的样品池实现气体的高效采样、光源的稳定激发，通过光学透镜组实现发射光的采集。针对发射光低强度短寿命的特点，设计了应用于光电倍增管的快速门控系统，避开了高强度激发光的干扰的同时，实现特定时序内的发射光的有效采集。结合光子计数技术对光子信号进行甄别测量，进而分析待测物浓度。The invention designs a special sample pool to realize high-efficiency sampling of gas, stable excitation of light source, and collection of emitted light through an optical lens group. Aiming at the low-intensity and short-life characteristics of emitted light, a fast gating system applied to photomultiplier tubes is designed to avoid the interference of high-intensity excitation light and achieve effective collection of emitted light within a specific time sequence. Combined with photon counting technology, the photon signal is screened and measured, and then the concentration of the analyte is analyzed.
本发明的主要特点如下：Main features of the present invention are as follows:
1、光源为高重频可调谐激光器，设计配套参比系统实现波长稳定输出。1. The light source is a high repetition frequency tunable laser, and a matching reference system is designed to achieve stable wavelength output.
2、样品池为低压密闭池，通过针孔完成采样，避免目标物的损耗，提高探测灵敏度。2. The sample pool is a low-pressure closed pool, and the sampling is completed through the pinhole to avoid the loss of the target and improve the detection sensitivity.
3、探测器为门控光电倍增管，设计高压调制电路和光电倍增管(PMT)分压电路，改变PMT不同打拿级上的加载电压，实现PMT的快速开启和响应恢复。3. The detector is a gated photomultiplier tube, and a high-voltage modulation circuit and a photomultiplier tube (PMT) voltage divider circuit are designed to change the loading voltage on different dynode levels of the PMT to achieve rapid turn-on and response recovery of the PMT.
4、采用光子计数卡实现超低强度激发光信号的光子检测，实现低浓度高活性自由基的测量。4. The photon counting card is used to realize the photon detection of the ultra-low intensity excitation light signal, and realize the measurement of low concentration and high activity free radicals.
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。对于实施例公开的系统而言，由于其与实施例公开的方法相对应，所以描述的比较简单，相关之处参见方法部分说明即可。Each embodiment in this specification is described in a progressive manner, each embodiment focuses on the difference from other embodiments, and the same and similar parts of each embodiment can be referred to each other. As for the system disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and for relevant details, please refer to the description of the method part.
本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处。综上所述，本说明书内容不应理解为对本发明的限制。In this paper, specific examples have been used to illustrate the principle and implementation of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core idea; meanwhile, for those of ordinary skill in the art, according to the present invention Thoughts, there will be changes in specific implementation methods and application ranges. In summary, the contents of this specification should not be construed as limiting the present invention.
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