WO2016029866A1 - 蒸发光散射检测器的鞘流装置 - Google Patents

蒸发光散射检测器的鞘流装置 Download PDF

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WO2016029866A1
WO2016029866A1 PCT/CN2015/088313 CN2015088313W WO2016029866A1 WO 2016029866 A1 WO2016029866 A1 WO 2016029866A1 CN 2015088313 W CN2015088313 W CN 2015088313W WO 2016029866 A1 WO2016029866 A1 WO 2016029866A1
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sheath flow
evaporation tube
sheath
light scattering
scattering detector
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PCT/CN2015/088313
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English (en)
French (fr)
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阎超
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阎超
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Priority to US15/036,416 priority Critical patent/US9829424B2/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Electro-optical investigation, e.g. flow cytometers
    • G01N15/1404—Fluid conditioning in flow cytometers, e.g. flow cells; Supply; Control of flow
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Electro-optical investigation, e.g. flow cytometers
    • G01N15/1456—Electro-optical investigation, e.g. flow cytometers without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals
    • G01N15/1459—Electro-optical investigation, e.g. flow cytometers without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals the analysis being performed on a sample stream
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Electro-optical investigation, e.g. flow cytometers
    • G01N15/1484—Electro-optical investigation, e.g. flow cytometers microstructural devices
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/84—Preparation of the fraction to be distributed
    • G01N15/1409—
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/84—Preparation of the fraction to be distributed
    • G01N2030/8447—Nebulising, aerosol formation or ionisation
    • G01N2030/8494—Desolvation chambers

Definitions

  • the present invention relates to an evaporative light scattering detector, and more particularly to a sheath flow device for evaporating a light scattering detector.
  • the Evaporative Light-Scattering Detector is a "universal” and “quality” detector. ELSD is not limited by the molecular structure of the substance itself, nor does it depend on the optical properties of the substance itself. As long as the volatility of the substance is lower than the volatility of the mobile phase solvent, it can be used for the analysis and detection of most non-volatile and semi-volatile substances. Especially in the detection of natural products, Chinese herbal medicines, lipids, surfactants and carbohydrates, and ELSD has little effect on the broadening of chromatographic peaks under nano-upflow, which is very suitable for the coupling of capillary micro-separation technology. use.
  • the Micro-fluid Evaporative Light-Scattering Detector ( ⁇ ELSD) is matched with the nanoliter to micro-upgrade liquid flow of the capillary separation system.
  • the principle is to atomize the capillary column elution solution.
  • the aerosol then evaporates the solvent on the surface of the aerosol in a heated evaporation tube, and finally the remaining non-volatile solute particles enter the light scattering detection cell, and the light beam emitted by the light source "impacts" the solute particles flowing through the detection cell to produce light scattering.
  • the optical signal is received by the photomultiplier tube and converted into an electrical signal.
  • the formed sample particles flow into the cavity of the light scattering detection cell, and the diffusion is small due to the small amount, so that the sample particle flow is difficult to flow.
  • the center of the beam emitted by the laser source reduces the sensitivity and stability of the detection; and the sample particle flow is also prone to eddy currents and turbulence in the cavity of the detection cell, which adversely affects the peak shape of the sample.
  • Sheath Flow is an auxiliary fluid, generally divided into Sheath Liquid and Sheath Gas, which essentially concentrates the sample fluid, such as sheath flow technology for flow cytometry. It can avoid the influence of blood cells flowing through the edge of the small hole and turbulence and eddy current.
  • a sheath flow device In the traditional ELSD instrument, a sheath flow device is also designed, but the structure of the conventional sheath flow device cannot achieve the ideal effect for the nano-upgrade to the micro-upgrade flow, and it cannot block the evaporation tube pair.
  • the heat transfer of the detection pool has an adverse effect on the detection module and cannot be adapted to the requirements of upgrading to micro-upgrade traffic.
  • a sheath flow device for evaporating a light scattering detector is provided.
  • a sheath flow device for an evaporative light scattering detector comprising an evaporation tube fixture, an evaporation tube insulation, a sheath flow nozzle flap, a sheath flow nozzle, a sheath flow sleeve, a sheath flow outlet member, and a stainless steel needle, the evaporation
  • the tube fixing member, the evaporation tube heat insulating member, the sheath flow nozzle blocking piece, the sheath flow nozzle, the sheath flow sleeve and the sheath flow outlet member are concentrically connected from front to back in order, and each of the six has a concentric inner hole, the evaporation
  • the inner diameter of the tube fixing member and the evaporation tube heat insulating member is the same as the outer diameter of the evaporation tube of the evaporative light scattering detector, and the inner hole inlet end of the sheath flow nozzle block has the same inner diameter as the outer diameter of the evaporation tube a step,
  • the evaporation tube fixing member, the evaporation tube heat insulating member, the sheath flow nozzle blocking piece and the sheath flow nozzle are all cylinders having the same outer diameter, the evaporation tube fixing member, the evaporation tube heat insulating member, the sheath flow nozzle blocking piece, and The sheath flow nozzles are sequentially concentrically connected by a fixing bolt, and the sheath flow nozzle is concentrically connected to the sheath flow sleeve by a fixing bolt.
  • the posterior side of the sheath flow sleeve has a recess that is concentric and that is adapted to the sheath flow outlet member, the sheath flow outlet member being secured within the recess.
  • the inner hole of the sheath flow sleeve is gradually extended from a wide section of the front portion to a narrow section of the rear portion, and is stepped.
  • the sheath flow carrier gas inlet passage is perpendicular to the inner bore of the sheath flow sleeve.
  • the sheath flow outlet member is detachably secured within the recess.
  • the evaporation tube heat insulating member is composed of three layers of heat insulating materials.
  • the evaporation tube heat insulation member is composed of a plastic layer, a rubber wood layer and a rubber cushion layer.
  • the stainless steel needle has an inner diameter of 1 mm to 5 mm and an outer diameter of 2 to 6 mm.
  • a sealing ring is disposed between the evaporation tube heat insulating member and the sheath flow nozzle blank, between the sheath flow nozzle blank and the sheath flow nozzle, and between the sheath flow nozzle and the sheath flow sleeve.
  • the effective encapsulation and convergence of the sheath carrier gas on the microparticle flow is realized, ensuring that the detection beam “impacts” on the center of the sample particle flow, improves the detection sensitivity, improves the peak shape of the sample, and enhances the stability of the instrument;
  • Figure 1 is a schematic view of the structure of the present invention
  • Figure 2 is a cross-sectional structural view of the present invention
  • Figure 3 is an experimental chromatogram of the sheath flow structure not installed
  • Figure 4 is an experimental chromatogram of the installation of the sheath flow device of the present invention.
  • Figure 5 is a graph of signal-to-noise ratio S/N as a function of sheath flow.
  • a sheath flow device for an evaporative light scattering detector includes an evaporation tube fixing member 110, an evaporation tube thermal insulation member 120, a sheath flow nozzle blocking piece 130, a sheath flow nozzle 140, and a sheath flow sleeve. 150, stainless steel needle 160 and sheath flow outlet member 170.
  • the evaporation tube fixing member 110, the evaporation tube thermal insulation member 120, the sheath flow nozzle blocking piece 130, the sheath flow nozzle 140, the sheath flow sleeve 150 and the sheath flow outlet member 170 are concentrically connected from front to back, and are concentric in each of the six. Inner hole.
  • the sheath flow nozzle blocking piece 130 A seal ring is disposed between the sheath flow nozzle 140 and the sheath flow nozzle 140 and the sheath flow sleeve 150.
  • the evaporation tube fixture 110, the evaporation tube insulation 120, the sheath flow nozzle block 130, and the sheath flow nozzle 140 are all cylinders having the same outer diameter.
  • the evaporation tube fixing member 110, the evaporation tube thermal insulation member 120, the sheath flow nozzle blocking piece 130, and the sheath flow nozzle 140 are sequentially concentrically connected by a fixing bolt, and the sheath flow nozzle 140 is concentrically connected to the sheath flow sleeve 150 by a fixing bolt, wherein
  • the rear side of the sheath flow sleeve 150 has a recess that is concentric and is adapted to the sheath flow outlet member 170, and the sheath flow outlet member 170 is secured within the recess.
  • the sheath flow outlet member 170 is detachably secured within the recess and the replacement sheath flow outlet member 170 can be adapted to match different outer diameter stainless steel needles 160.
  • the inner diameter of the evaporation tube holder 110 and the evaporation tube insulation 120 is the same as the outer diameter of the evaporation tube 2 of the evaporative light scattering detector.
  • the evaporating tube heat insulation member 120 can effectively insulate between the evaporation tube 2 and the detection pool of the evaporative light scattering detector, prevent excessive evaporation of the sample aerosol, and reduce the influence of the evaporation temperature on the detection pool module, which is composed of three layers.
  • the heat insulating material is compositely composed. Preferably, it is composed of a plastic layer, a rubber wood layer and a rubber mat layer, and the compounding order is not limited.
  • the inner bore inlet end of the sheath flow nozzle flap 130 has the same inner barrier step as the outer diameter of the evaporation tube 2.
  • the inner hole 141 of the sheath flow nozzle 140 has a front width and a narrow horn shape, and the inner diameter of the inlet end is the same as the inner diameter of the outlet end of the inner hole of the sheath flow nozzle 130, and the inner diameter of the outlet end is the same as the inner diameter of the stainless steel needle 160.
  • the sheath flow sleeve 150 has a sheath carrier gas inlet channel 151 communicating with the inner hole thereof, and the sheath carrier gas has a cleaning effect on the detection chamber cavity, thereby effectively reducing the baseline noise of the evaporative light scattering detector under the microfluidic system and improving The signal to noise ratio of the microdetection signal.
  • the sheath flow carrier gas inlet passage 151 is perpendicular to the inner bore of the sheath flow sleeve 150.
  • the inner hole of the sheath flow sleeve 150 gradually extends from the wide section of the front portion to the narrow section of the rear portion, and is stepped.
  • the front end of the stainless steel needle 160 is inserted into the outlet end of the inner hole of the sheath flow nozzle 140, and the rear end thereof extends through the inner hole of the sheath flow sleeve 150 into the inner hole of the sheath flow outlet member 170, and the sheath flow
  • the outlet end of the inner hole of the outlet member 170 is flush.
  • the stainless steel needle 160 has an inner diameter of 1 mm to 5 mm and an outer diameter of 2 to 6 mm.
  • the inner diameter of the sheath flow outlet member 170 is slightly larger than the outer diameter of the stainless steel needle 160, and an outlet annulus of the sheath carrier gas is formed therebetween for controlling the linear flow rate of the sheath carrier gas to achieve optimal experimental conditions. Replacing the sheath flow outlet member 170 and matching the stainless steel needles 160 of different outer diameters can create a variety of annulus conditions.
  • the eluent of the capillary column passes through the atomization system of the evaporative light scattering detector to form an aerosol into the evaporation tube 2, and the surface of the aerosol moves in the evaporation tube 2
  • the solvent is evaporated, and the remaining non-volatile sample particles are driven by the carrier gas into the sheath flow device of the present invention; the heat from the evaporation tube 2 is first blocked by the evaporation tube insulation 120, and the sample particles flow through the sheath flow nozzle.
  • the flap 130 enters the stainless steel needle 160 through the outlet end of the flared inner bore of the sheath flow nozzle 140, and at the same time, the sheath carrier gas (pure air or nitrogen) enters the channel 151 from the sheath carrier gas on the sheath flow sleeve 150 into the sheath.
  • the inner hole of the flow sleeve 150 then enters the light scattering detection cell from the outlet annulus formed by the stainless steel needle 160 and the sheath flow outlet member 170, and at the same time, the sample particle flow flowing out from the end of the stainless steel needle 160 is wrapped and converged.
  • the sample particle flow that is converged and wrapped is irradiated by the light beam emitted by the light source in the detection pool to form light scattering, and the light scattering signal is collected by the detection module, converted and transmitted to a computer, and finally the detection chromatogram is obtained.
  • the effective encapsulation and convergence of the sheath carrier gas on the microparticle flow ensures that the detection beam “impacts” on the center of the sample particle flow, improves the detection sensitivity, improves the peak shape of the sample, and enhances the stability of the instrument.
  • This experiment is the detection of glucose by an evaporative light scattering detector.
  • Atomized carrier gas flow rate 0.40L/min, high purity N2;
  • Atomized carrier gas pressure 5.40 bar;
  • Evaporation tube size 12mm I.D.*25cm long;
  • Sheath flow rate 0-3.0 L/min.
  • Figure 3 shows the chromatogram of the glucose sample obtained by directly connecting the detection tank without continuous installation of the sheath flow structure. It can be seen that there is tailing and bulging after the peak of the sample, and the RSD6 values of the peak area and the peak height are respectively The peak area and peak height were poorly repeatable at 23.41% and 23.76%.
  • Figure 4 is a chromatogram of the glucose sample obtained by continuously injecting six needles under the condition of a sheath flow rate of 1.0 L/min after installing the sheath flow device of the present invention. It can be seen that the sheath flow device of the present invention can improve the glucose sample well.
  • the peak shape eliminates the phenomenon of trailing bulging after the peak, and the RSD6 values of peak area and peak height are 1.80% and 1.89%, respectively, and the stability and precision of the instrument are significantly improved.
  • Fig. 5 is a graph showing the signal-to-noise ratio S/N as a function of sheath flow, showing that the sheath flow device has a significant effect on the signal-to-noise ratio of the microfluidic evaporative photodetector, and that there is an optimal sheath flow condition.

Abstract

一种蒸发光散射检测器的鞘流装置，包括蒸发管固定件（110）、蒸发管隔热件（120）、鞘流喷嘴挡片（130）、鞘流喷嘴（140）、鞘流套（150）、鞘流出口件（170）以及不锈钢喷针（160），所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片、鞘流喷嘴、鞘流套以及鞘流出口件由前至后依次同心连接，且六者内均具有同心的内孔。所述装置适用于纳升级到微升级流量的ELSD鞘流装置，一方面对进入检测池的物质颗粒流进行包裹聚集，减少了涡流、湍流的形成，改善了样品色谱峰形，增强了样品检测的稳定性，另一方面对检测池起到清洗作用，降低了基线噪音，提高了信噪比。

Description

蒸发光散射检测器的鞘流装置 技术领域
本发明涉及蒸发光散射检测器，尤其涉及一种蒸发光散射检测器的鞘流装置。
背景技术
蒸发光散射检测器(Evaporative Light-Scattering Detector，ELSD),是一种“通用型”和“质量型”检测器。ELSD不受物质本身分子结构的限制,也不依赖物质本身的光学特性,只要物质的挥发性低于流动相溶剂的挥发性，就可用于绝大多数不挥发和半挥发性物质的分析检测，尤其在天然产物、中草药、脂类、表面活性剂及碳水化合物等物质的检测方面表现出巨大优势，并且ELSD对纳升级流量下色谱峰展宽的影响很小，非常适合于毛细管微分离技术的联用。
微流蒸发光散射检测器(Micro-fluid Evaporative Light-Scattering Detector，μELSD)正是与毛细管分离体系的纳升至微升级液体流量相匹配，其原理是先将毛细管色谱柱洗脱液雾化形成气溶胶，然后在加热的蒸发管中将气溶胶表面的溶剂蒸发，最后余下的不挥发性溶质颗粒进入光散射检测池中，光源发射光束“撞击”流经检测池的溶质颗粒产生光散射作用，由光电倍增管接受光信号并将其转化成电信号。
由于毛细管分离体系的微量特性，毛细管色谱柱的洗脱液经过雾化、蒸发后，形成的样品颗粒流入光散射检测池空腔时，因量少易产生扩散，使得样品颗粒流较难流经激光光源发射的光束中心，从而降低检测灵敏度和稳定性；而且样品颗粒流在检测池空腔中还易形成涡流、湍流，对样品色谱峰形产生不利影响。
鞘流(Sheath Flow)是一种辅助性流体，一般分为鞘液(Sheath Liquid)和鞘气(Sheath Gas)，其本质是使得样品流体更加汇聚，如鞘流技术用于流式细胞仪，可避免计数中血细胞从小孔边缘处流过及湍流，涡流的影响。
传统的ELSD仪器设备中，也设计有鞘流装置，但是针对纳升级到微升级流量，传统鞘流装置的结构并不能达到理想作用，其无法阻隔蒸发管对 检测池的热传递，对检测模块产生了不良影响，并且无法适应纳升级到微升级流量的要求。
发明内容
基于此，针对上述技术问题，提供一种蒸发光散射检测器的鞘流装置。
为解决上述技术问题，本发明采用如下技术方案：
一种蒸发光散射检测器的鞘流装置，包括蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片、鞘流喷嘴、鞘流套、鞘流出口件以及不锈钢喷针，所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片、鞘流喷嘴、鞘流套以及鞘流出口件由前至后依次同心连接，且六者内均具有同心的内孔，所述蒸发管固定件以及蒸发管隔热件的内孔与蒸发光散射检测器的蒸发管外径相同，所述鞘流喷嘴挡片的内孔入口端具有与所述蒸发管的外径相同的阻挡内台阶，所述鞘流喷嘴的内孔呈后宽前窄的喇叭状，其入口端的内径与所述鞘流喷嘴挡片内孔出口端的内径相同，其出口端内径与所述不锈钢喷针的内径相同，所述鞘流套上具有与其内孔连通的鞘流载气进入通道，所述不锈钢喷针的前端插设于所述鞘流喷嘴内孔的出口端内，其后端穿过所述鞘流套的内孔伸入于所述鞘流出口件的内孔中，且与该鞘流出口件内孔的出口端齐平，所述鞘流出口件的内径略大于所述不锈钢喷针的外径，两者之间形成鞘流载气的出口环隙。
所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片以及鞘流喷嘴均为外径相同的圆柱体，所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片以及鞘流喷嘴通过固定螺栓依次同心连接，所述鞘流喷嘴通过固定螺栓与所述鞘流套同心连接。
所述鞘流套的后侧面具有同心且与所述鞘流出口件适配的凹槽，所述鞘流出口件固定于所述凹槽内。
所述鞘流套的内孔由前部的宽段逐渐延伸至后部的窄段，呈阶梯状。
所述鞘流载气进入通道与所述鞘流套的内孔垂直。
所述鞘流出口件可拆卸的固定于所述凹槽内。
所述蒸发管隔热件由三层隔热材料复合构成。
所述蒸发管隔热件由塑料层、胶木板层以及橡胶垫层复合构成。
所述不锈钢喷针的内径为1mm-5mm，其外径为2-6mm。
所述蒸发管隔热件与鞘流喷嘴挡片之间、鞘流喷嘴挡片与所述鞘流喷嘴之间、鞘流喷嘴与所述鞘流套之间均设有密封圈。
本发明一种蒸发光散射检测器的鞘流装置具有以下优点：
1、实现了蒸发管与检测池间的有效隔热，防止样品气溶胶的过度蒸发，并同时减小蒸发温度对检测池模块的影响；
2、实现了鞘流载气对微小颗粒流的有效包裹和会聚，确保检测光束“撞击”在样品颗粒流的中心，提高了检测灵敏度，改善了样品峰形，增强了仪器稳定性；
3、通过可拆卸的鞘流出口件，实现对鞘流参数的有效控制，确保最佳实验条件；
4、通过鞘流载气对检测池腔体的清洗作用，有效降低微流体系下蒸发光散射检测器的基线噪音，提高微检测信号的信噪比。
附图说明
下面结合附图和具体实施方式本发明进行详细说明：
图1为本发明的结构示意图；
图2为本发明的剖视结构示意图；
图3为未安装鞘流结构的实验色谱图；
图4为安装本发明鞘流装置的实验色谱图；
图5为信噪比S/N随鞘流流量变化的曲线图。
具体实施方式
如图1以及图2所示，一种蒸发光散射检测器的鞘流装置，包括蒸发管固定件110、蒸发管隔热件120、鞘流喷嘴挡片130、鞘流喷嘴140、鞘流套150、不锈钢喷针160以及鞘流出口件170。
蒸发管固定件110、蒸发管隔热件120、鞘流喷嘴挡片130、鞘流喷嘴140、鞘流套150以及鞘流出口件170由前至后依次同心连接，且六者内均具有同心的内孔。
其中，蒸发管隔热件120与鞘流喷嘴挡片130之间、鞘流喷嘴挡片130 与鞘流喷嘴140之间、鞘流喷嘴140与鞘流套150之间均设有密封圈。
蒸发管固定件110、蒸发管隔热件120、鞘流喷嘴挡片130以及鞘流喷嘴140均为外径相同的圆柱体。
具体地，蒸发管固定件110、蒸发管隔热件120、鞘流喷嘴挡片130以及鞘流喷嘴140通过固定螺栓依次同心连接，鞘流喷嘴140通过固定螺栓与鞘流套150同心连接，其中，鞘流套150的后侧面具有同心且与鞘流出口件170适配的凹槽，鞘流出口件170固定于凹槽内。
鞘流出口件170可拆卸的固定于上述凹槽内，更换鞘流出口件170可匹配不同外径的不锈钢喷针160。
蒸发管固定件110以及蒸发管隔热件120的内孔与蒸发光散射检测器的蒸发管2外径相同。
蒸发管隔热件120可实现蒸发光散射检测器的蒸发管2与检测池间的有效隔热，防止样品气溶胶的过度蒸发，同时减小蒸发温度对检测池模块的影响，其由三层隔热材料复合构成，较佳的，其由塑料层、胶木板层以及橡胶垫层复合构成，复合次序不限。
鞘流喷嘴挡片130的内孔入口端具有与蒸发管2的外径相同的阻挡内台阶。
鞘流喷嘴140的内孔141呈前宽后窄的喇叭状，其入口端的内径与鞘流喷嘴挡片130内孔出口端的内径相同，其出口端内径与不锈钢喷针160的内径相同。
鞘流套150上具有与其内孔连通的鞘流载气进入通道151，通过鞘流载气对检测池腔体具有清洗作用，可有效降低微流体系下蒸发光散射检测器的基线噪音，提高微检测信号的信噪比。
较佳的，鞘流载气进入通道151与鞘流套150的内孔垂直。
其中，鞘流套150的内孔由前部的宽段逐渐延伸至后部的窄段，呈阶梯状。
不锈钢喷针160的前端插设于鞘流喷嘴140内孔的出口端内，其后端穿过鞘流套150的内孔伸入于鞘流出口件170的内孔中，且与该鞘流出口件170内孔的出口端齐平。
其中，不锈钢喷针160的内径为1mm-5mm，其外径为2-6mm。
鞘流出口件170的内径略大于不锈钢喷针160的外径，两者之间形成鞘流载气的出口环隙，用于控制鞘流载气的线性流速，以达到最佳实验条件，通过更换鞘流出口件170，并匹配不同外径的不锈钢喷针160，可以形成多种环隙条件。
本发明的具体工作过程如下：
毛细管色谱柱的洗脱液(含流动相和样品，简称洗脱液)，经过蒸发光散射检测器的雾化系统，形成气溶胶进入蒸发管2，气溶胶在蒸发管2内运动时，表面的溶剂被蒸发，余下不挥发的样品颗粒在载气的带动下，进入本发明鞘流装置；蒸发管2带来的热量首先被蒸发管隔热件120所隔断，样品颗粒流经过鞘流喷嘴挡片130，通过鞘流喷嘴140喇叭形内孔的出口端进入不锈钢喷针160，同时，鞘流载气(纯净空气或氮气)由鞘流套150上的鞘流载气进入通道151进入鞘流套150的内孔中，然后从不锈钢喷针160与鞘流出口件170构成的出口环隙中进入光散射检测池，并同时对从不锈钢喷针160末端流出的样品颗粒流进行包裹会聚，被会聚包裹的样品颗粒流在检测池内被光源发出的光束照射形成光散射，通过检测模块对光散射信号进行采集，转换并传输至计算机，最终得到检测色谱图，其中，鞘流载气对微小颗粒流的有效包裹和会聚，确保了检测光束“撞击”在样品颗粒流的中心，提高了检测灵敏度，改善了样品峰形，增强了仪器稳定性。
为了验证本发明鞘流装置对蒸发光散射检测器的作用，本实施例进行了如下实验：
本实验为蒸发光散射检测器对葡萄糖的检测。
实验条件：
雾化载气流量：0.40L/min，高纯N2；
雾化载气压力：5.40bar；
蒸发管尺寸：12mm I.D.*25cm长；
蒸发温度：30℃；
流动相：纯水；
柱流速：900nL/min；
样品：1×10-2g/mL葡萄糖；
进样量：20nL；
鞘流流量：0-3.0L/min。
图3为没有安装鞘流结构时，直接连接检测池，连续进样六针所得葡萄糖样品色谱图，可以看出，样品峰后有拖尾和鼓包现象，其峰面积和峰高的RSD6值分别为23.41％和23.76％，峰面积和峰高的重复性差。
图4为安装本发明鞘流装置后，鞘流流量为1.0L/min的条件下，连续进样六针所得葡萄糖样品色谱图，可以看出，本发明鞘流装置可以很好的改善葡萄糖样品峰形，消除了峰后拖尾鼓包现象，其峰面积和峰高的RSD6值分别为1.80％和1.89％，仪器稳定性和精密度显著提高。
图5为信噪比S/N随鞘流流量变化的曲线图，表明鞘流装置对微流蒸发光检测器的信噪比有显著的提高作用，且存在最佳鞘流条件。
但是，本技术领域中的普通技术人员应当认识到，以上的实施例仅是用来说明本发明，而并非用作为对本发明的限定，只要在本发明的实质精神范围内，对以上所述实施例的变化、变型都将落在本发明的权利要求书范围内。

Claims (7)

  1. 一种蒸发光散射检测器的鞘流装置，其特征在于，包括蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片、鞘流喷嘴、鞘流套、鞘流出口件以及不锈钢喷针，所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片、鞘流喷嘴、鞘流套以及鞘流出口件由前至后依次同心连接，且六者内均具有同心的内孔，所述蒸发管固定件以及蒸发管隔热件的内孔与蒸发光散射检测器的蒸发管外径相同，所述鞘流喷嘴挡片的内孔入口端具有与所述蒸发管的外径相同的阻挡内台阶，所述鞘流喷嘴的内孔呈前宽后窄的喇叭状，其入口端的内径与所述鞘流喷嘴挡片内孔出口端的内径相同，其出口端内径与所述不锈钢喷针的内径相同，所述鞘流套上具有与其内孔连通的鞘流载气进入通道，所述不锈钢喷针的前端插设于所述鞘流喷嘴内孔的出口端内，其后端穿过所述鞘流套的内孔伸入于所述鞘流出口件的内孔中，且与该鞘流出口件内孔的出口端齐平，所述鞘流出口件的内径略大于所述不锈钢喷针的外径，两者之间形成鞘流载气的出口环隙。
  2. 根据权利要求1所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片以及鞘流喷嘴均为外径相同的圆柱体，所述蒸发管固定件、蒸发管隔热件、鞘流喷嘴挡片以及鞘流喷嘴通过固定螺栓依次同心连接，所述鞘流喷嘴通过固定螺栓与所述鞘流套同心连接。
  3. 根据权利要求1或2所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述鞘流套的后侧面具有同心且与所述鞘流出口件适配的凹槽，所述鞘流出口件固定于所述凹槽内。
  4. 根据权利要求3所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述鞘流出口件可拆卸的固定于所述凹槽内。
  5. 根据权利要求4所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述蒸发管隔热件由三层隔热材料复合构成。
  6. 根据权利要求5所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述蒸发管隔热件由塑料层、胶木板层以及橡胶垫层复合构成。
  7. 根据权利要求6所述的一种蒸发光散射检测器的鞘流装置，其特征在于，所述不锈钢喷针的内径为1mm-5mm，其外径为2-6mm。
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