技术领域technical field
本实用新型涉及安全检测技术领域，具体地，涉及一种检测设备。The utility model relates to the technical field of safety detection, in particular to a detection device.
背景技术Background technique
离子迁移谱仪(IMS)是目前国际上主流的痕量检测设备之一，IMS技术主要依据不同离子在弱电场作用下的迁移率的差异来对样品进行分离鉴别，它具有结构简单，灵敏度高，分析速度快以及结果可靠等特点，可以在线快速检测毒品、爆炸物、毒气和生化气体等，被广泛用于军事(化学战剂监测)、民事(反恐、缉毒等)等众多领域，在维护国家安全、维持社会稳定、加强国防力量、维系国计民生等方面发挥着巨大的作用。然而，采用单独的IMS检测多种成分的复杂混合物检测时，却容易发生漏报、误报。因此，以提高分析仪器分辨能力为目的的各种联用技术如雨后春笋般应运而生。其中，气相色谱-离子迁移谱(GC-IMS)联用技术利用GC突出的分离特点和IMS快速响应、高灵敏度的优势有效地解决了GC低鉴别能力和IMS对混合物进行检测时存在的交叉灵敏度(cross sensitivity)问题，并可获取色谱保留时间、漂移时间和信号强度的三维谱图，能够有效的分辨出成分复杂的样品，检测限优于ppb量级，分辨时间从几分钟到几十分钟。与其它联用技术相比，GC-IMS具有接口简单，维护费用低，性价比高等诸多特点，因而，近年来GC-IMS联用技术得到了迅猛发展，并在小型化及便携式方面体现出了充分的优势，大力发展快速GC-IMS检测技术将是未来安全检测技术的重要发展方向之一。Ion mobility spectrometer (IMS) is one of the mainstream trace detection equipment in the world at present. IMS technology mainly separates and identifies samples based on the difference in the mobility of different ions under the action of a weak electric field. It has a simple structure and high sensitivity. , fast analysis speed and reliable results, etc. It can quickly detect drugs, explosives, poisonous gas and biochemical gases online, and is widely used in military (chemical warfare agent monitoring), civil (anti-terrorism, anti-drug, etc.) and many other fields. It plays a huge role in national security, maintaining social stability, strengthening national defense, and maintaining the national economy and people's livelihood. However, when a single IMS is used to detect a complex mixture of multiple components, it is prone to false negatives and false negatives. Therefore, various combined techniques for the purpose of improving the resolution of analytical instruments have sprung up like mushrooms after rain. Among them, gas chromatography-ion mobility spectrometry (GC-IMS) combined technology uses the outstanding separation characteristics of GC and the advantages of fast response and high sensitivity of IMS to effectively solve the cross-sensitivity existing in the low discrimination ability of GC and the detection of mixtures by IMS. (cross sensitivity) problem, and can obtain the three-dimensional spectrum of chromatographic retention time, drift time and signal intensity, and can effectively distinguish samples with complex components. The detection limit is better than ppb level, and the resolution time is from several minutes to tens of minutes. . Compared with other combined technologies, GC-IMS has many characteristics such as simple interface, low maintenance cost, and high cost performance. Therefore, GC-IMS combined technology has developed rapidly in recent years, and has fully demonstrated its miniaturization and portability. It is one of the important development directions of future security detection technology to vigorously develop fast GC-IMS detection technology.
进样装置是IMS不可或缺的部分，进样装置和进样方法的好坏不 仅会影响仪器的使用范围而且还会影响仪器对被检物质的响应难度和精度。对于单独的IMS，具有多种进样器与之相匹配，技术较为成熟。对于单独的GC，一般采用顶空进样方式，省去了复杂的样品前处理(适合于快速检测)，但顶空进样仍需“破坏性”的获取一定量的样品，因此它不适合不拆包情形下的痕量气体现场快检。The sampling device is an integral part of the IMS. The quality of the sampling device and the sampling method will not only affect the scope of use of the instrument but also affect the difficulty and accuracy of the instrument's response to the tested substance. For a single IMS, there are a variety of sample injectors to match it, and the technology is relatively mature. For a separate GC, headspace sampling is generally used, which saves complicated sample pretreatment (suitable for rapid detection), but headspace sampling still needs to "destructively" obtain a certain amount of samples, so it is not suitable On-site quick detection of trace gas without unpacking.
实用新型内容Utility model content
本实用新型的目的是提供一种检测设备，其克服现有技术中诸多不足。根据本实用新型一方面的检测设备包括采样装置，用于采集将要被检测的样品；预处理进样装置，用于对来自采样装置的样品预处理；和，样品分析装置，用于分离来自预处理进样装置的被预处理的样品和分析分离后的样品。The purpose of the utility model is to provide a detection device, which overcomes many deficiencies in the prior art. A detection device according to one aspect of the present invention includes a sampling device for collecting a sample to be detected; a pretreatment sampling device for preprocessing a sample from the sampling device; and a sample analysis device for separating the samples from the pretreatment Processing of preconditioned samples and analysis of separated samples from the sampling device.
根据本实用新型的一方面，采样装置包括：腔体，具有位于腔体的第一端的吸入样品的采样入口和位于腔体的与第一端相对的第二端附近的用于排出样品的样品出口；腔体还包括位于腔体的壁内的充气入口和排气口，According to one aspect of the present invention, the sampling device includes: a cavity, with a sampling inlet positioned at a first end of the cavity for sucking in a sample and a port for discharging a sample near a second end opposite to the first end of the cavity. a sample outlet; the chamber also includes an inflation inlet and an exhaust port located in the walls of the chamber,
其中充气入口配置成向腔体内吹入气流，排气口配置成排出气体，以便与充气入口一起在腔体内形成龙卷风式气流，所述龙卷风式气流沿从腔体的第一端至第二端螺旋式前进。Wherein the inflation inlet is configured to blow air into the cavity, and the exhaust port is configured to discharge gas, so that together with the inflation inlet, a tornado air flow is formed in the cavity, and the tornado air flow is from the first end to the second end of the cavity. spiral forward.
根据本实用新型的一方面，部分腔体的内壁被形成为截头圆锥形形状，截头圆锥形内壁的小直径圆形端靠近腔体的采样入口，并且截头圆锥形内壁的大直径圆形端靠近样品出口。According to an aspect of the present invention, the inner wall of part of the cavity is formed in a frusto-conical shape, the small-diameter circular end of the frusto-conical inner wall is close to the sampling inlet of the cavity, and the large-diameter circular end of the frusto-conical inner wall The shaped end is near the sample outlet.
根据本实用新型的一方面，充气入口配置成使得充气入口的轴向进气方向与腔体内壁的内表面接近相切，并且充气入口的轴向进气方向向样品出口侧倾斜。According to one aspect of the present invention, the gas inlet is configured such that the axial inlet direction of the gas inlet is nearly tangent to the inner surface of the inner wall of the cavity, and the axial inlet direction of the gas inlet is inclined to the sample outlet side.
根据本实用新型的一方面，排气口配置成排出在腔体内形成的龙卷风式气流的外围气体。According to an aspect of the present invention, the exhaust port is configured to discharge peripheral air of the tornado airflow formed in the cavity.
根据本实用新型的一方面，排气口的开口方向接近排气口处的气流的速度方向的反向。According to an aspect of the present invention, the opening direction of the exhaust port is close to the opposite direction of the velocity direction of the airflow at the exhaust port.
根据本实用新型的一方面，采样装置还包括设置在腔体的第二端的混合腔部分，样品被送入混合腔部分通过进样口送入检测系统。According to an aspect of the present invention, the sampling device further includes a mixing chamber part arranged at the second end of the chamber body, and the sample is sent into the mixing chamber part and sent into the detection system through the sample inlet.
根据本实用新型的一方面，混合腔部分通过半透膜与腔体其他部分隔开。According to an aspect of the present invention, part of the mixing chamber is separated from other parts of the chamber by a semi-permeable membrane.
根据本实用新型的一方面，混合腔部分设置载气通道以向混合腔部分注入载气以便与样品混合。According to an aspect of the present invention, the mixing chamber part is provided with a carrier gas channel for injecting the carrier gas into the mixing chamber part so as to mix with the sample.
根据本实用新型的一方面，采样装置还包括位于第一端的过滤网，过滤网用于阻挡大颗粒物质进入采样入口，所述过滤网包括具有刚性的过滤大颗粒的粗滤网和过滤微颗粒的细滤网。According to an aspect of the present utility model, the sampling device also includes a filter screen at the first end, the filter screen is used to prevent large particles from entering the sampling inlet, and the filter screen includes a rigid coarse filter screen and a fine filter screen for filtering large particles. Fine mesh for particles.
根据本实用新型的一方面，采样装置还包括用于控制腔体内温度的控温系统，包括设置在腔体的壁内的用于升温的加热器和用于测量温度的温度传感器。According to an aspect of the present invention, the sampling device further includes a temperature control system for controlling the temperature in the cavity, including a heater for raising the temperature and a temperature sensor for measuring the temperature arranged in the wall of the cavity.
根据本实用新型的一方面，采样装置还包括包围腔体的壁的保温层。According to an aspect of the present invention, the sampling device further includes an insulating layer surrounding walls of the cavity.
根据本实用新型的一方面，采样装置还包括与充气入口连通的充气泵和与排气口连通的排气泵，其中排气泵流速是充气泵的10倍或更高。According to an aspect of the present invention, the sampling device further includes an air pump communicated with the air inlet and an exhaust pump communicated with the exhaust port, wherein the flow rate of the exhaust pump is 10 times or higher than that of the air pump.
根据本实用新型的一方面，预处理进样装置包括：活塞式吸附器，具有能够与采样装置连通的吸附腔，该吸附腔被配置成吸附由采样装置采集的样品；活塞缸，限定用于容纳活塞式吸附器并与吸附腔连通的活塞腔；热解析腔，与吸附腔和活塞腔连通并被配置成热解析被吸附在吸附腔内的样品；和泵，通过导管与活塞腔连通并被配置成通过样品采集结构将泄漏到环境气体中的样品抽吸到吸附腔，According to one aspect of the present invention, the pretreatment sampling device includes: a piston-type adsorber, which has an adsorption chamber capable of communicating with the sampling device, and the adsorption chamber is configured to absorb the sample collected by the sampling device; a piston cylinder is defined for a piston chamber housing the piston adsorber and communicating with the adsorption chamber; a thermal desorption chamber communicating with the adsorption chamber and the piston chamber and configured to thermally desorb a sample adsorbed in the adsorption chamber; and a pump communicating with the piston chamber through a conduit and configured to draw sample leaked into the ambient gas through the sample collection structure into the adsorption chamber,
其中，活塞式吸附器被构造成能够在样品采集位置和样品解析位置之间在活塞腔内移动，在样品采集位置中吸附腔定位在热解析腔外并与样品采集结构连通以吸附由样品采集结构采集的样品，在样品解析位置中吸附腔定位在热解析腔内使得所吸附的样品在热解析腔内被热解析。Wherein, the piston-type adsorber is configured to be able to move in the piston cavity between the sample collection position and the sample analysis position. For the sample collected by the structure, the adsorption cavity is positioned in the thermal analysis cavity in the sample analysis position so that the adsorbed sample is thermally analyzed in the thermal analysis cavity.
根据本实用新型的一方面，活塞缸包括安装在热解析腔上的缸体，缸体上设置有与活塞腔连通的采样连接气嘴，连接管的一端被构 造成密封地和可拆卸地安装在采样连接气嘴中。According to one aspect of the utility model, the piston cylinder includes a cylinder body installed on the thermal analysis chamber, the cylinder body is provided with a sampling connection nozzle communicating with the piston chamber, and one end of the connecting pipe is configured to be sealed and detachably installed In the sampling connection gas nozzle.
根据本实用新型的一方面，连接管内放置有用于吸收所采集的样品中的水分的干燥剂。According to one aspect of the present invention, a desiccant for absorbing moisture in the collected samples is placed in the connecting tube.
根据本实用新型的一方面，连接管的至少一个部分包括可伸缩软管。According to an aspect of the present invention, at least a portion of the connection pipe includes a telescopic hose.
根据本实用新型的一方面，活塞式吸附器包括活塞杆体和连接至活塞杆体的末端的吸附腔，并且吸附腔包括内部填充有吸附剂的网状结构。According to an aspect of the present invention, the piston type adsorber includes a piston rod body and an adsorption chamber connected to an end of the piston rod body, and the adsorption chamber includes a mesh structure filled with an adsorbent inside.
根据本实用新型的一方面，吸附腔包括吸附通道，该吸附通道被构造成在活塞式吸附器位于样品采集位置中时与采样装置连通以接收所采集的样品。According to an aspect of the present invention, the adsorption chamber includes an adsorption channel configured to communicate with the sampling device to receive collected samples when the piston adsorber is located in the sample collection position.
根据本实用新型的一方面，活塞式吸附器还包括可拆卸地连接至吸附腔的远离活塞杆体的一端的隔热垫。According to an aspect of the present invention, the piston-type adsorber further includes a heat insulation pad detachably connected to the end of the adsorption chamber away from the piston rod body.
根据本实用新型的一方面，活塞杆体包括冷却通道和形成在活塞杆体的下部中的多个通孔，冷却通道被构造成在活塞式吸附器位于样品采集位置中时直接与环境气体连通，并在活塞式吸附器位于样品解析位置中时通过形成在活塞缸中的冷却通孔与环境气体连通，并且所述多个通孔被构造成与冷却通道和活塞腔连通。According to an aspect of the present invention, the piston rod body includes a cooling channel and a plurality of through holes formed in the lower part of the piston rod body, the cooling channel is configured to directly communicate with the ambient gas when the piston-type adsorber is located in the sample collection position, and When the piston adsorber is in the sample analysis position, it communicates with the ambient gas through cooling through holes formed in the piston cylinder, and the plurality of through holes are configured to communicate with the cooling channel and the piston cavity.
根据本实用新型的一方面，检测设备还包括多个密封圈，所述多个密封圈围绕活塞式吸附器设置使得活塞式吸附器能够被密封地容纳在活塞缸内。According to an aspect of the present invention, the detection device further includes a plurality of sealing rings arranged around the piston absorber so that the piston absorber can be hermetically accommodated in the piston cylinder.
根据本实用新型的一方面，活塞缸包括设置在热解析腔内以引导活塞式吸附器在热解析腔内的运动的导轨。According to an aspect of the present invention, the piston cylinder includes a guide rail arranged in the thermal analysis chamber to guide the movement of the piston-type adsorber in the thermal analysis chamber.
根据本实用新型的一方面，热解析腔包括腔体和设置在腔体的内壁内的衬管，并且腔体的外壁包覆有加热结构。According to an aspect of the present invention, the thermal analysis chamber includes a chamber body and a liner arranged in the inner wall of the chamber body, and the outer wall of the chamber body is covered with a heating structure.
根据本实用新型的一方面，热解析腔还设置有载气入口、出气口和分析仪器接口。According to an aspect of the utility model, the thermal analysis chamber is further provided with a carrier gas inlet, a gas outlet and an analysis instrument interface.
根据本实用新型的一方面，检测设备还包括设置在活塞缸和热解析腔之间的隔热结构。According to an aspect of the present invention, the detection device further includes a heat insulation structure arranged between the piston cylinder and the thermal analysis chamber.
根据本实用新型的一方面，预处理进样装置包括：吸气泵、吸附 器、活塞缸体和解析缸体，所述解析缸体具有解析腔，所述解析缸体设有与所述解析腔连通载气入口、载气吹扫/分流出口以及连接分析仪器的接口，所述解析缸体的外壁设有加热膜和温度传感器；所述活塞缸体设有两个活塞腔，每个所述活塞腔安装一个所述吸附器；所述活塞缸体安装在所述解析缸体上，且两个所述活塞腔均与所述解析腔相连通；所述活塞缸体设有均与两个所述活塞腔连通的样品进气口和吸气泵气口，所述样品进气口与采样装置连接，所述吸气泵气口与所述吸气泵连接；所述吸附器包括相连接的吸附筛筒和活塞杆，所述吸附筛筒用于存放吸附剂；所述活塞杆可滑动安装在所述活塞腔中，带动所述吸附筛筒沿所述活塞腔滑动并可伸入所述解析腔中，且所述吸附筛筒可同时与所述样品进气口和吸气泵气口连通。According to one aspect of the present invention, the pretreatment sampling device includes: an air suction pump, an adsorber, a piston cylinder, and an analysis cylinder, the analysis cylinder has an analysis cavity, and the analysis cylinder is provided with the analysis chamber. The cavity is connected to the carrier gas inlet, the carrier gas purge/splitting outlet and the interface connected to the analysis instrument. The outer wall of the analytical cylinder is provided with a heating film and a temperature sensor; the piston cylinder is provided with two piston chambers, each of which is One of the adsorbers is installed in the piston chamber; the piston cylinder is installed on the analysis cylinder, and the two piston chambers are all connected with the analysis chamber; the piston cylinder is provided with both The sample air inlet and the aspirator pump air port communicated with the two piston chambers, the sample air inlet is connected with the sampling device, and the aspirator pump air port is connected with the aspirator pump; the adsorber includes connected Adsorption sieve cylinder and piston rod, the adsorption sieve cylinder is used to store the adsorbent; the piston rod can be slidably installed in the piston cavity, driving the adsorption sieve cylinder to slide along the piston cavity and extend into the in the analysis chamber, and the adsorption sieve can be communicated with the sample inlet and the air inlet of the aspirator at the same time.
根据本实用新型的一方面，所述解析缸体的外壁还设有温度传感器和保温层。According to one aspect of the present invention, the outer wall of the analytical cylinder is further provided with a temperature sensor and a thermal insulation layer.
根据本实用新型的一方面，所述吸附筛筒设有一个吸附筛口，所述吸附筛口可与所述样品进气口连通。According to an aspect of the present utility model, the adsorption sieve cylinder is provided with an adsorption sieve, and the adsorption sieve can communicate with the sample inlet.
根据本实用新型的一方面，每个所述活塞腔设有一个冷却气口，所述冷却气口设有入口阀门；所述活塞杆设有冷却空腔，所述冷却空腔可与冷却气口连通，且所述活塞杆的侧壁设有与冷却空腔连接的通风孔，所述通风孔可与吸气泵气口连通。According to an aspect of the utility model, each of the piston chambers is provided with a cooling air port, and the cooling air port is provided with an inlet valve; the piston rod is provided with a cooling cavity, and the cooling cavity can communicate with the cooling air port. And the side wall of the piston rod is provided with a ventilation hole connected to the cooling cavity, and the ventilation hole can communicate with the air port of the suction pump.
根据本实用新型的一方面，所述吸附筛筒的底部设置一个绝热垫。According to an aspect of the present utility model, a heat insulating pad is arranged at the bottom of the adsorption screen drum.
根据本实用新型的一方面，所述吸附器与所述活塞腔之间设有多个密封圈。According to an aspect of the present utility model, a plurality of sealing rings are provided between the adsorber and the piston cavity.
根据本实用新型的一方面，所述解析缸体的内壁设有衬管。According to one aspect of the present utility model, the inner wall of the analysis cylinder is provided with a liner.
根据本实用新型的一方面，所述活塞缸体与所述解析缸体之间设有隔热盘。According to an aspect of the present utility model, a heat insulating plate is provided between the piston cylinder and the analysis cylinder.
根据本实用新型的一方面，所述解析缸体还设有一个载气吹扫/分流接口。According to an aspect of the utility model, the analysis cylinder is further provided with a carrier gas purge/splitting interface.
根据本实用新型的一方面，样品分析装置包括样品导入装置，样品导入装置包括：集束毛细管柱，由非金属材料形成的多个毛细管柱 构成，具有入口端和出口端；和，温控系统，与集束毛细管柱结合用于控制集束毛细管柱内的温度；样品分析装置还包括离子迁移谱分析装置，离子迁移谱分析装置用于分析样品导入装置导入的样品，所述离子迁移谱分析装置包括用于气体反应的腔，腔具有用于导入样品的样品导入口，其中，非金属材料形成的集束毛细管柱的出口端通过离子迁移谱分析装置的样品导入口直接插入离子迁移谱分析装置的腔内。According to one aspect of the present invention, the sample analysis device includes a sample introduction device, and the sample introduction device includes: a bundled capillary column, composed of a plurality of capillary columns formed of non-metallic materials, having an inlet port and an outlet port; and, a temperature control system, Combined with the clustered capillary column, it is used to control the temperature in the clustered capillary column; the sample analysis device also includes an ion mobility spectrometry analysis device, and the ion mobility spectrometry analysis device is used to analyze the sample introduced by the sample introduction device, and the ion mobility spectrometry analysis device includes The gas reaction chamber has a sample inlet for introducing samples, wherein the outlet end of the clustered capillary column formed of non-metallic materials is directly inserted into the chamber of the ion mobility spectrometry device through the sample inlet of the ion mobility spectrometry device .
根据本实用新型的一方面，样品分析装置还包括隔热定位装置，配置成能够在样品导入装置和离子迁移谱分析装置之间连接样品导入装置和离子迁移谱分析装置，并且隔断样品导入装置和离子迁移谱分析装置之间的热传递，以便样品导入装置和离子迁移谱分析装置的分别的独立温度控制。According to an aspect of the present utility model, the sample analysis device further includes a thermal insulation positioning device configured to connect the sample introduction device and the ion mobility spectrometry analysis device between the sample introduction device and the ion mobility spectrometry analysis device, and isolate the sample introduction device from the ion mobility spectrometry analysis device. Heat transfer between the ion mobility spectrometry device for separate independent temperature control of the sample introduction device and the ion mobility spectrometry device.
根据本实用新型的一方面，隔热定位装置包括与样品导入装置的出口端连接的第一连接端和与离子迁移谱分析装置连接的第二连接端，第一连接端密封集束毛细管柱的一个端部，第二连接端的形状与离子迁移分析装置的腔的开口的形状互补。According to one aspect of the present utility model, the thermal insulation positioning device includes a first connection end connected to the outlet end of the sample introduction device and a second connection end connected to the ion mobility spectrometer analysis device, and the first connection end seals one of the bundled capillary columns. The shape of the end, the second connection end, is complementary to the shape of the opening of the cavity of the ion mobility analysis device.
根据本实用新型的一方面，隔热定位装置由耐高温和绝热性能良好的塑料材料形成，如PEEK，聚四氟乙烯等。According to one aspect of the present invention, the heat-insulating positioning device is made of plastic materials with high temperature resistance and good heat-insulating performance, such as PEEK, polytetrafluoroethylene and the like.
根据本实用新型的一方面，样品导入装置还包括配置成包围并保护集束毛细管柱的金属圆套，集束毛细管柱的金属圆套的长度配置成当集束毛细管柱插入到离子迁移谱分析装置的腔内时金属圆套不进入离子迁移谱分析装置的样品导入口。According to an aspect of the present invention, the sample introduction device further includes a metal sleeve configured to surround and protect the clustered capillary column. When inside, the metal sleeve does not enter the sample introduction port of the ion mobility spectrometer analysis device.
根据本实用新型的一方面，样品导入装置的温控系统包括导热体，导热体配置成直接接触包围集束毛细管柱的金属圆套，以及嵌入在导热体内的至少一个加热器和至少一个传感器。According to an aspect of the present invention, the temperature control system of the sample introduction device includes a thermal conductor configured to directly contact the metal sleeve surrounding the bundled capillary column, and at least one heater and at least one sensor embedded in the thermal conductor.
根据本实用新型的一方面，导热体包括导热体外周上的多个凸起，在多个凸起之间能够形成用于布置流体通道或流过流体的空间。According to an aspect of the present invention, the heat conductor includes a plurality of protrusions on the periphery of the heat conductor, and spaces for arranging fluid passages or flowing fluid can be formed between the plurality of protrusions.
根据本实用新型的一方面，热媒流体管道蜿蜒穿过多个凸起的方式或以螺旋地围绕导热体的方式穿过多个凸起之间，以便热媒流体管道与导热体之间热传递。According to one aspect of the present invention, the heat medium fluid pipe meanders through a plurality of protrusions or passes between the plurality of protrusions in a manner that spirally surrounds the heat conductor, so that there is a gap between the heat medium fluid pipe and the heat conductor. heat transfer.
根据本实用新型的一方面，样品导入装置还包括外壳，外壳包围温控系统。According to an aspect of the present invention, the sample introduction device further includes a casing, and the casing surrounds the temperature control system.
根据本实用新型的一方面，样品导入装置还包括保温层，保温层布置在外壳和导热体之间。According to an aspect of the present invention, the sample introduction device further includes an insulating layer, and the insulating layer is arranged between the shell and the heat conductor.
根据本实用新型的一方面，保温层通过导热体上的多个凸起支撑。According to one aspect of the present invention, the insulation layer is supported by a plurality of protrusions on the heat conductor.
根据本实用新型的一方面，离子迁移谱分析装置为包括正离子迁移管和负离子迁移管的正、负双模式离子迁移管，离子迁移谱分析装置包括电离区，配置成将被通入的载气电离成反应离子并将反应离子送入反应区，其中电离区设置在离子迁移谱分析装置的与集束毛细管柱的出口端的相对的一侧。According to one aspect of the present invention, the ion mobility spectrometry analysis device is a positive and negative dual-mode ion transfer tube including a positive ion transfer tube and a negative ion transfer tube. The gas is ionized into reactant ions and the reactant ions are sent into a reaction zone, wherein the ionization zone is disposed on the opposite side of the ion mobility spectrometry device from the outlet end of the clustered capillary column.
本实用新型的检测设备可以实现对气载物质的放大收集，采样效率大大提高，能实现不需开包在现场对携带的易挥发性、半挥发性及表面沾染的痕量物质进行集采样、进样、检测；这种一站式的检测技术既提高了检测速度又能避免安检中的隐私纷争，工作原理像嗅探犬，非常适合于机场、海关等的现场快速检测需求；用于表面沾染样品及气体样品的取、进样快速检测，在免拆包的条件下实现样品的快速收集、预浓缩解析以及分离，大大提高了分析的精确性，节省了样品溶液制备时间；尤其体现在有多个被检物品时，可在对前一个被检物进行分析的同时对下一个待检物进行采样和富集，节约了样品采集检测总时长，能有效的提高分析仪器的吞吐量和检测速度，节约了成本；通过对样品进行浓缩可以降低对检测器(如IMS、MS、DMS)检测下限的要求，降低了仪器的开发难度及成本，同时还能降低仪器的误报率；有利于仪器向小型化和便携式发展；集束毛细管柱分离的成分直接进入双模式迁移管中间的反应区，避开了电离区，既实现了避免产生分子离子碎片的目的，又实现了气相色谱-离子迁移谱分析装置联用谱仪同时鉴别正负离子的功能，使谱仪同时对正负电亲和性的大分子都能响应，弥补了以往技术的不足，拓宽了集束毛细管柱-离子迁移谱分析装置对检测物质的选择性；集束毛细管柱-离子迁移谱分析装置的接口不需要转接单元，集束毛细管柱端口直接和离子迁移 谱分析装置相耦合，避免因转接单元转弯而发生湍流，能有效提到离子迁移谱分析装置的检测灵敏度和分辨率；集束毛细管柱和离子迁移谱分析装置反应区基座之间设计隔热定位装置，同时兼具集束毛细管柱的定位和绝热作用，结构简单，便于安装操作，省去了增设额外的转接单元及其温控系统设计；集束毛细管柱的加热器件均匀嵌套在热导套内，这样设计的好处在于既能实现了集束毛细管柱快速升温又保证了集束毛细管柱受热均匀，保证样品气化分离均匀，减少分离歧视；热导套、散热管道、加热器件、泵，以及控制器的配合控制实现了集束毛细管柱的程序升温功能，可将集束毛细管柱-离子迁移谱分析装置联用谱仪的应用领域拓展到应对宽沸程样品成分的分离，提高了对分析物质的选择性。The detection equipment of the utility model can realize the amplification and collection of airborne substances, greatly improve the sampling efficiency, and can collect and sample the volatile, semi-volatile and surface-contaminated trace substances carried on site without opening the package. Sample injection and detection; this one-stop detection technology not only improves the detection speed but also avoids privacy disputes in security checks. It works like a sniffer dog and is very suitable for on-site rapid detection needs at airports, customs, etc.; used for surface Contaminated samples and gas samples are taken and injected quickly, and samples can be quickly collected, pre-concentrated, analyzed and separated without unpacking, which greatly improves the accuracy of analysis and saves the time for sample solution preparation; especially in When there are multiple inspected objects, the next object to be inspected can be sampled and enriched while the previous inspected object is analyzed, which saves the total time of sample collection and detection, and can effectively improve the throughput and throughput of the analytical instrument. The detection speed saves the cost; by concentrating the sample, the requirements for the detection limit of the detector (such as IMS, MS, DMS) can be reduced, the difficulty and cost of the development of the instrument can be reduced, and the false alarm rate of the instrument can also be reduced; It is conducive to the development of miniaturized and portable instruments; the components separated by the cluster capillary column directly enter the reaction zone in the middle of the dual-mode transfer tube, avoiding the ionization zone, which not only achieves the purpose of avoiding the generation of molecular ion fragments, but also realizes gas chromatography-ion The mobility spectrometry analysis device is combined with the spectrometer to identify positive and negative ions at the same time, so that the spectrometer can respond to both positive and negative electrophilic macromolecules, which makes up for the shortcomings of previous technologies and broadens the scope of clustered capillary column-ion mobility spectrometry analysis. The selectivity of the device to the detection substance; the interface of the cluster capillary column-ion mobility spectrometry analysis device does not need a transfer unit, and the port of the cluster capillary column is directly coupled with the ion mobility spectrometry device to avoid turbulent flow due to the turning of the transfer unit, which can Effectively improve the detection sensitivity and resolution of the ion mobility spectrometer analysis device; a thermal insulation positioning device is designed between the cluster capillary column and the base of the reaction zone of the ion mobility spectrometer analysis device, and has both the positioning and heat insulation functions of the cluster capillary column, and the structure is simple , easy to install and operate, eliminating the need to add an additional adapter unit and its temperature control system design; the heating device of the clustered capillary column is evenly nested in the heat conduction sleeve, the advantage of this design is that it can realize the rapid temperature rise of the clustered capillary column It also ensures that the clustered capillary column is heated evenly, ensures that the sample is vaporized and separated uniformly, and reduces separation discrimination; the coordinated control of the thermal conductivity sleeve, heat dissipation pipe, heating device, pump, and controller realizes the temperature program function of the clustered capillary column, which can The application field of the combined spectrometer of the cluster capillary column-ion mobility spectrometer is expanded to deal with the separation of components of samples with a wide boiling range, which improves the selectivity of the analyte.
附图说明Description of drawings
图1示出根据本实用新型的检测设备的示意图。Fig. 1 shows a schematic diagram of a detection device according to the present invention.
图2示出根据本实用新型一个实施例的检测设备的采样装置的示意图。Fig. 2 shows a schematic diagram of a sampling device of a detection device according to an embodiment of the present invention.
图3示出根据本实用新型一个实施例的气帘引导体的截面示意图。Fig. 3 shows a schematic cross-sectional view of an air curtain guide body according to an embodiment of the present invention.
图4示出根据本实用新型一个实施例的采样装置底端面管线引出口示意图。图5示出根据本实用新型一个实施例的预处理进样装置的示意图。Fig. 4 shows a schematic diagram of a pipeline outlet on the bottom end surface of the sampling device according to an embodiment of the present invention. Fig. 5 shows a schematic diagram of a pretreatment sampling device according to an embodiment of the present invention.
图6示出根据本实用新型一个实施例的预处理进样装置的活塞式吸附器的结构的示意图。Fig. 6 shows a schematic diagram of the structure of the piston adsorber of the pretreatment sampling device according to an embodiment of the present invention.
图7示出根据本实用新型一个实施例的预处理进样装置的示意图，其中预处理进样装置处于解析进样状态。Fig. 7 shows a schematic diagram of a pretreatment sample introduction device according to an embodiment of the present invention, wherein the pretreatment sample introduction device is in an analytical sample introduction state.
图8示出根据本实用新型一个实施例的另一预处理进样装置的示意图。Fig. 8 shows a schematic diagram of another pretreatment sampling device according to an embodiment of the present invention.
图9示出根据本实用新型一个实施例的样品分析装置的示意图。Fig. 9 shows a schematic diagram of a sample analysis device according to an embodiment of the present invention.
图10是根据本实用新型的一个实施例的样品分析装置的沿A-A 线的截面图；Figure 10 is a cross-sectional view along line A-A of a sample analysis device according to an embodiment of the present invention;
图11是根据本实用新型的一个实施例的样品分析装置的沿B-B和C-C线的截面图；Fig. 11 is a cross-sectional view along B-B and C-C lines of a sample analysis device according to an embodiment of the present invention;
图12是根据本实用新型的一个实施例的样品分析装置的导热体上的多个凸起以及流体管道在多个凸起之间的布置。Fig. 12 shows a plurality of protrusions on the heat conductor of the sample analysis device according to an embodiment of the present invention and the arrangement of fluid pipes between the plurality of protrusions.
具体实施方式Detailed ways
尽管本实用新型容许各种修改和可替换的形式，但是它的具体的实施例通过例子的方式在附图中示出，并且将详细地在本文中描述。然而，应该理解，随附的附图和详细的描述不是为了将本实用新型限制到公开的具体形式，而是相反，是为了覆盖落入由随附的权利要求限定的本实用新型的精神和范围中的所有的修改、等同形式和替换形式。附图是为了示意，因而不是按比例地绘制的。While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will be described herein in detail. It should be understood, however, that the accompanying drawings and detailed description are not intended to limit the invention to the precise form disclosed, but on the contrary, are intended to cover within the spirit and scope of the invention as defined by the appended claims. All modifications, equivalents, and alternatives within the scope. The drawings are for illustration purposes and are not drawn to scale.
下面根据附图说明根据本实用新型的多个实施例。A number of embodiments according to the present utility model are described below according to the accompanying drawings.
如图1所示，根据本实用新型的一个实施例，提供一种检测设备，包括：采样装置100，用于采集将要被检测的样品；预处理进样装置200、300，用于对来自采样装置的样品进行预处理；样品分析装置400，用于分离来自预处理进样装置100的被预处理的样品和分析分离后的样品。采样装置100、预处理进样装置200、300以及样品分析装置400可以通过例如波纹管连接并连通。图1中示出的检测设备的各个部分的布置是为了示意而不是限制。As shown in Figure 1, according to an embodiment of the present utility model, a detection device is provided, including: a sampling device 100 for collecting samples to be detected; pretreatment sampling devices 200, 300 for sampling from The sample of the device is pretreated; the sample analysis device 400 is used to separate the pretreated sample from the pretreatment sampling device 100 and analyze the separated sample. The sampling device 100 , the pretreatment sampling devices 200 , 300 and the sample analysis device 400 may be connected and communicated through, for example, bellows. The arrangement of the various parts of the detection device shown in FIG. 1 is for illustration and not limitation.
下面将对检测设备的多个部分分别进行详细的介绍。Multiple parts of the detection equipment will be introduced in detail below.
图2是根据本实用新型的检测设备的一个实施例的采样装置100的纵剖面示意图。根据本实用新型的实施例的龙卷风式的采样装置对气载物质具有放大的收集功能，其能够实时采样。采样装置100包括：端盖101，具有孔；和，布置在端盖101上的压环102，压环102将粗滤网103和微滤网104安装在端盖101的开孔上面，以阻挡大颗粒物质进入采样装置100内部。粗滤网不但可以过滤大的颗粒，而且具有较强的刚性，可以阻止来自外部环境的压力以及大颗粒的撞击。微 滤网用于过滤细小的固体微粒或微颗粒。备选地，可以使用一体的端盖101，其中一体的端盖具有开口，或称为采样入口，并且采样入口布置有多孔元件103或104，以便阻挡大颗粒物质通过该端盖101。Fig. 2 is a schematic longitudinal sectional view of a sampling device 100 according to an embodiment of the detection device of the present invention. The tornado-type sampling device according to the embodiment of the present invention has an amplified collection function for airborne substances, and it can sample in real time. The sampling device 100 includes: an end cover 101 with a hole; and, a pressure ring 102 arranged on the end cover 101, the pressure ring 102 installs the coarse filter screen 103 and the micro filter screen 104 on the opening of the end cover 101 to prevent Large particulate matter enters the sampling device 100 interior. The coarse filter can not only filter large particles, but also has strong rigidity, which can prevent the pressure from the external environment and the impact of large particles. Microfilters are used to filter fine solid particles or particles. Alternatively, an integral end cap 101 with an opening, or sampling inlet, arranged with a porous element 103 or 104 to block passage of large particulate matter through the end cap 101 may be used.
根据本实用新型的采样装置100还包括气帘引导体105，端盖101可以通过O型密封圈108封盖在旋转式的气帘引导体105的上面，以便将气帘引导体105的上环面密封。旋转式气帘引导体105具有圆筒式外侧壁，并且可以具有如图所示的截面呈漏斗形的内侧壁。换句话说，气帘引导体105可以是一个圆筒及其内一个漏斗式内侧壁的组合。备选地，气帘引导体105可以是一体形成的单件。漏斗式内侧壁与圆筒式外侧壁的夹角可以在20°-30°之间，然而其他夹角也是可选的。气帘引导体105的漏斗式内侧壁的下端面的直径至少是上端面直径的两倍。换句话说，漏斗式内侧壁形成的下开口的直径至少是上开口的直径的两倍。这种漏斗形的设计用于模拟形成龙卷风。气帘引导体105的漏斗式内侧壁的内侧面限定内部空间，即如图2所示的截面图中，两个如图所示的内侧壁之间的内部空间。The sampling device 100 according to the present invention also includes an air curtain guide 105, and the end cover 101 can be sealed on the rotating air curtain guide 105 by an O-ring 108, so as to seal the upper ring surface of the air curtain guide 105. The rotary air curtain guide 105 has a cylindrical outer sidewall, and may have a funnel-shaped inner sidewall in cross-section as shown. In other words, the air curtain guide body 105 may be a combination of a cylinder and a funnel-shaped inner sidewall. Alternatively, the air curtain guide 105 may be an integrally formed single piece. The included angle between the funnel-shaped inner wall and the cylindrical outer wall can be between 20°-30°, but other included angles are also optional. The diameter of the lower end surface of the funnel-shaped inner side wall of the air curtain guide body 105 is at least twice the diameter of the upper end surface. In other words, the diameter of the lower opening formed by the funneled inner sidewall is at least twice the diameter of the upper opening. This funnel-shaped design is used to simulate the formation of a tornado. The inner side of the funnel-shaped inner sidewall of the air curtain guide body 105 defines an inner space, that is, the inner space between two inner sidewalls as shown in the sectional view shown in FIG. 2 .
图3示出气帘引导体105的侧壁沿A-A的横截面示意图。如图3所示，气帘引导体105的漏斗式内侧壁的上端均匀布置多个旋流孔106，这些旋流孔106的轴向方向与漏斗的内侧壁接近相切，旋流孔106的轴线与竖直方向的夹角在45°-90°之间。由此，旋流孔沿与气帘引导体105的漏斗式内侧壁相切并且向下(沿图2中示出的箭头方向)朝向，使得气体从旋流孔流出且沿漏斗式内侧壁相切的方向向下流动。FIG. 3 shows a schematic cross-sectional view of the side wall of the air curtain guide 105 along A-A. As shown in Figure 3, a plurality of swirl holes 106 are evenly arranged on the upper end of the funnel-type inner wall of the air curtain guide body 105, and the axial direction of these swirl holes 106 is nearly tangent to the inner wall of the funnel, and the axis of the swirl holes 106 The included angle with the vertical direction is between 45°-90°. Thus, the swirl holes are oriented tangentially to the funnel-shaped inner sidewall of the air curtain guide 105 and downward (in the direction of the arrow shown in FIG. direction of downward flow.
在气帘引导体105的圆筒式外侧壁上有充气入口107。旋转气帘引导体105的圆筒式外侧壁、漏斗式内侧壁以及端盖101包围一个环形空间。气体可以从充气入口107进入环形空间，然后环形空间的空气沿漏斗式内侧壁上的旋流孔106吹进气帘引导体105的漏斗形内部空间内，形成旋流气帘130。There is an air inlet 107 on the cylindrical outer wall of the air curtain guide body 105 . The cylindrical outer wall, the funnel inner wall and the end cap 101 of the rotating air curtain guide body 105 enclose an annular space. Gas can enter the annular space from the inflation inlet 107 , and then the air in the annular space is blown into the funnel-shaped inner space of the air curtain guide body 105 along the swirl holes 106 on the funnel-shaped inner wall to form a swirl air curtain 130 .
在本实施例中，示出的是样品从上端吸入，从下端排出，充气气体气流从上向下螺旋流动。然而，这只是一个示例，当采样装置100水平放置对着被检测物体时，例如采样入口对着位于采样装置100左 边的被检测物体时，气帘引导体105的小口一侧对着左侧被检测物体，此时漏斗形内壁109是横置的布置形式，样品从左向右前进。In this embodiment, it is shown that the sample is sucked in from the upper end and discharged from the lower end, and the inflation gas flow spirally flows from the top to the bottom. However, this is only an example. When the sampling device 100 is placed horizontally against the object to be detected, for example, when the sampling inlet faces the object to be detected on the left side of the sampling device 100, the side of the small opening of the air curtain guide body 105 is placed against the left side. Objects are detected. At this time, the funnel-shaped inner wall 109 is arranged horizontally, and the sample advances from left to right.
根据本实用新型的实施例，气帘引导体105可以包括充气管道118。图2示出一种布置方式，充气管道118一端与充气入口107连通，另一端与充气用的气泵128连通。充气用的气泵128将空气风沿充气管道118过充气入口107送进环形空间，环形空间的空气风沿漏斗式内侧壁上的旋流孔106吹进漏斗形内部空间内形成旋流气帘130。According to an embodiment of the present invention, the air curtain guide 105 may include an inflation duct 118 . FIG. 2 shows an arrangement. One end of the inflation pipeline 118 communicates with the inflation inlet 107 , and the other end communicates with the air pump 128 for inflation. The air pump 128 used for inflation sends the air wind into the annular space along the inflation pipe 118 through the inflation inlet 107, and the air wind in the annular space is blown into the funnel-shaped inner space along the swirl hole 106 on the funnel-shaped inner wall to form a swirl air curtain 130.
采样装置100还包括导风腔109，导风腔具有圆柱形内壁。导风腔109通过O型密封圈嵌套在气帘引导体105下面。导风腔109与气帘引导体105可以以其他形式接合，只要不影响在导风腔中形成龙卷风式气流即可。龙卷风式气流是本领域技术人员已知的，即在气流的外围气体高速或至少快速地螺旋地旋转，即在横向截面上(在本实施例中导风腔的截面上)是旋转运动，同时在纵向方向上具有向前(在本实施例中从采样入口的一端至样品出口一端)运动的速度；同时气流中心或轴心处气体沿纵向方向向前被抽吸。导风腔109用于维持龙卷风式气旋并引导龙卷风式轴心吸吮的气载物质进入后续检测器件。如图2所示，旋流气帘130向下推进，进入导风腔109形成旋流气流131。龙卷风式旋转气流32沿着导风腔109流动，经导风腔109下端侧壁上的旋风出口110从排气泵接口123以及经排风口127排出。气泵接口123本身就是一个排风口，为了增大排风速度可以在底端面多设计几个排风口，在图4中示意地示出排风口127，排风口127可以设置在面对旋流气流131的外围出气流134的任意位置，它可以和123相对应，可以是一个也可以是多个，这个排风口127没有在图2中画出来。The sampling device 100 also includes an air guide chamber 109, which has a cylindrical inner wall. The air guide cavity 109 is nested under the air curtain guide body 105 through an O-ring. The air guide chamber 109 and the air curtain guide body 105 can be joined in other forms, as long as it does not affect the formation of a tornado-like airflow in the air guide chamber. The tornado airflow is known to those skilled in the art, that is, the peripheral gas in the airflow rotates helically at a high speed or at least rapidly, that is, on the transverse section (on the section of the wind guide cavity in this embodiment) it is a rotational movement, and at the same time In the longitudinal direction, there is a speed of moving forward (from one end of the sampling inlet to one end of the sample outlet in this embodiment); at the same time, the gas at the center or axis of the airflow is sucked forward along the longitudinal direction. The air guide cavity 109 is used to maintain the tornado cyclone and guide the airborne material sucked by the tornado axis to enter the subsequent detection device. As shown in FIG. 2 , the swirl air curtain 130 pushes down and enters the air guide chamber 109 to form a swirl airflow 131 . The tornado-type rotating airflow 32 flows along the air guide chamber 109 , and is discharged from the exhaust pump interface 123 and the air outlet 127 through the cyclone outlet 110 on the lower side wall of the air guide chamber 109 . The air pump interface 123 itself is an air exhaust port. In order to increase the exhaust air speed, several more air exhaust ports can be designed on the bottom surface. The air exhaust port 127 is schematically shown in Fig. 4, and the air exhaust port 127 can be arranged on the face Any position of the airflow 134 on the periphery of the swirling airflow 131 can correspond to 123, and there can be one or more. The air outlet 127 is not shown in FIG. 2 .
采样装置100还包括漏斗形底盖113，其通过O型密封圈108将导风腔109下端面口盖封。底盖113和导风腔109下端口之间设有半透膜111，半透膜111可以阻止吸入气载物质中的水分子、氨分子以及其他杂质污染物进入并污染后端的色谱柱或迁移管。此外，半透膜111还有限制团簇的形成，进而提高仪器的分辨率。The sampling device 100 also includes a funnel-shaped bottom cover 113 , which seals the lower end surface of the air guiding cavity 109 through an O-ring 108 . A semi-permeable membrane 111 is provided between the bottom cover 113 and the lower port of the air guide cavity 109, and the semi-permeable membrane 111 can prevent water molecules, ammonia molecules and other impurity pollutants inhaled from the airborne substance from entering and contaminating the back-end chromatographic column or migrating Tube. In addition, the semipermeable membrane 111 also limits the formation of clusters, thereby improving the resolution of the instrument.
根据本实用新型的实施例，可以设置两片网状金属112，以便对半透膜111进行夹持保护，使半透膜112免受气流冲破。According to an embodiment of the present invention, two pieces of mesh metal 112 may be provided to clamp and protect the semi-permeable membrane 111 and prevent the semi-permeable membrane 112 from being broken by the airflow.
漏斗形底盖113可以作为载气和样品的混合区或混合腔。漏斗形底盖113可以包括载气通道121，用于注入载气，进来的载气在漏斗中与样品充分混合。漏斗形底盖113还可以包括进样口120，采集的样品与载气例如在混合预热后通过进样口120排出，进入下一级分析装置。在某些情况下，样品和载气可以直接混合不需要加热而排出。The funnel-shaped bottom cover 113 can serve as a mixing area or chamber for carrier gas and sample. The funnel-shaped bottom cover 113 may include a carrier gas channel 121 for injecting carrier gas, and the incoming carrier gas is fully mixed with the sample in the funnel. The funnel-shaped bottom cover 113 may also include a sample inlet 120 , and the collected sample and carrier gas are discharged through the sample inlet 120 after being mixed and preheated, and enter the next-stage analysis device. In some cases, the sample and carrier gas can be mixed directly and discharged without heating.
采样装置100还包括设置在导风腔109上的保温套114，设置在导风腔109内的加热棒116以及温度传感器117，由此它们构成温控系统，可以对导风腔109进行控温，例如加热升温。温控系统可将腔体内的温度控制在50℃-250℃，高温有助于高沸点的气载物质快速气化并顺利通过半透膜，并且有利于气化样品和从漏斗式侧壁上的载气通道121进来的载气在漏斗中充分混合，能有效提高仪器对高沸点物质的检测极限。采集的样品与载气混合预热后被载气携带进入进样口120。旋转气帘引导体105、导风腔109、底盖113可采用热性能好的金属材料，其外保温套113可采用～10mm厚的气凝胶或玻璃或陶瓷棉。可选地，可以采用聚四氟乙烯外罩115套罩在保温层114外。Sampling device 100 also comprises the insulation cover 114 that is arranged on the air guide chamber 109, the heating rod 116 that is arranged in the air guide chamber 109 and temperature sensor 117, thus they constitute temperature control system, can carry out temperature control to air guide chamber 109 , such as heating up. The temperature control system can control the temperature in the chamber between 50°C and 250°C. The high temperature helps the airborne substances with high boiling point to vaporize quickly and pass through the semi-permeable membrane smoothly, and it is also conducive to vaporizing the sample and removing it from the funnel side wall. The carrier gas coming in from the carrier gas channel 121 is fully mixed in the funnel, which can effectively improve the detection limit of the instrument for high boiling point substances. The collected sample is mixed with the carrier gas and preheated, and then carried by the carrier gas into the sample inlet 120 . The rotating air curtain guide body 105, the air guide cavity 109, and the bottom cover 113 can be made of metal materials with good thermal performance, and the outer heat preservation jacket 113 can be made of ~10mm thick airgel or glass or ceramic wool. Optionally, a polytetrafluoroethylene outer cover 115 can be used to cover the insulation layer 114 .
外罩115的底端面可以设置包括充气泵接口122、排气泵接口123、GC柱/离子迁移管接口124、加热棒引出线125、温度传感器引出线26、排风口127以及载气管接口136，见图4所示。其中，充气泵接口122和排气泵接口123可以分别接一个气泵128，用于持续提供气体压力以便在采样装置100内部形成龙卷风式气流。排气泵接口123期望布置成使得气阻尽可能小，因而排气泵接口在导风腔内的开口期望迎着气流的方向，使得气流容易地流入排气泵接口。排气泵接口123也可以不接气泵128直接用作排风口。为了使龙卷风式吸引放大的气流排出，可以多设计几个排风口127。GC柱/离子迁移管接口124可以接预处理装置200或300，也可以接GC柱，也可以直接接离子迁移管。载气管接口136接分子筛135以便使得载气得到净化。The bottom surface of the outer cover 115 can be provided with an air pump interface 122, an exhaust pump interface 123, a GC column/ion transfer tube interface 124, a heating rod lead-out line 125, a temperature sensor lead-out line 26, an air exhaust port 127 and a carrier gas pipe interface 136, see Figure 4 shows. Wherein, the air pump interface 122 and the exhaust pump interface 123 can be respectively connected with an air pump 128 for continuously providing gas pressure so as to form a tornado-like airflow inside the sampling device 100 . The exhaust pump interface 123 is expected to be arranged so that the air resistance is as small as possible, so the opening of the exhaust pump interface in the air guide chamber is expected to face the direction of the airflow, so that the airflow can easily flow into the exhaust pump interface. The exhaust pump interface 123 can also be directly used as an air exhaust port without connecting the air pump 128 . In order to make the airflow amplified by the tornado-like suction exhaust, several more air outlets 127 can be designed. The GC column/ion transfer tube interface 124 can be connected to the pretreatment device 200 or 300, or can be connected to a GC column, or directly connected to the ion transfer tube. The carrier gas pipe interface 136 is connected to a molecular sieve 135 to purify the carrier gas.
如图所示的气泵128的功率可按需调节。由于龙卷风式具有气体收集放大功能，排气泵的流速是充气泵的10倍以上。The power of the air pump 128 as shown can be adjusted as needed. Because the tornado type has the function of gas collection and amplification, the flow rate of the exhaust pump is more than 10 times that of the air pump.
为了避免充气泵128充入的空气流对从采样目标133上吸吮的目标成分造成干扰，一方面可以将充气泵采集的空气源距离采样目标133尽可能远，如可用能伸缩转向的软导管将气泵和采样端孔拉开距离，另一方面可以对进入充气泵的空气进行过滤净化，避免气体交叉污染，提高采样仪器的定位采样的灵敏性。In order to prevent the air flow charged by the air pump 128 from interfering with the target components sucked from the sampling target 133, on the one hand, the air source collected by the air pump can be as far away as possible from the sampling target 133, such as a soft conduit that can be retracted and turned. The distance between the air pump and the sampling port hole is widened. On the other hand, the air entering the air pump can be filtered and purified to avoid gas cross-contamination and improve the sensitivity of the sampling instrument for positioning and sampling.
以下说明根据本实用新型的实施例的对气体具有放大收集功能的龙卷风式采样装置100的采样、进样过程。The following describes the sampling and sampling process of the tornado sampling device 100 with the function of amplifying and collecting gas according to the embodiment of the present utility model.
将本实用新型的采样装置100的前端孔在5-10cm的地方对准采样目标133，同时打开充气和排气气泵128。充气气流129沿充气管通过充气入口107充入气帘引导体105的环形空间内，在气泵128的持续的风压下在环形空间内产生气体压力，在气压作用下，空气沿气帘引导体105上的旋流孔106吹进漏斗内部空间内，由于旋流孔106的特定构造，空气沿特定方向吹入内部空间中，由此形成漏斗形旋转气帘130。在气泵128的不断吹入空气的情况下，不断形成的旋转气帘130沿着导风腔109内壁移动，即，绕导风腔109的中心轴线132快速旋转并同时向下移动，形成龙卷风式气流131。由于旋转形成的离心力的作用，龙卷风式气流的中心气压显著地减小，例如，中心轴线132的气压比周围气压低大约10倍，由此在导风腔109的中心轴线处将产生很大的抽吸力。抽吸力可使得被采样的目标133附近内的气载物质从导风腔109的前端孔周围被吸入导风腔109的风轴中心附近，并形成样品气柱，沿龙卷风式气流的中心轴线132向下移动，最终样品到达进样半透膜111。这个过程类似于自然界中龙卷风式的“龙取水”的现象。Aim the front hole of the sampling device 100 of the present invention at the sampling target 133 at a distance of 5-10 cm, and simultaneously turn on the inflation and exhaust air pump 128 . The inflation airflow 129 is filled into the annular space of the air curtain guide body 105 through the inflation inlet 107 along the inflation pipe, and the gas pressure is generated in the annular space under the continuous wind pressure of the air pump 128. The swirl holes 106 are blown into the inner space of the funnel, and due to the specific configuration of the swirl holes 106, air is blown into the inner space in a specific direction, thereby forming a funnel-shaped swirling air curtain 130 . When the air pump 128 continuously blows in air, the continuously formed rotating air curtain 130 moves along the inner wall of the air guide chamber 109, that is, it rotates rapidly around the central axis 132 of the air guide chamber 109 and moves downward at the same time, forming a tornado air flow 131. Due to the centrifugal force formed by the rotation, the central air pressure of the tornado airflow significantly reduces, for example, the air pressure of the central axis 132 is about 10 times lower than the ambient air pressure, thus a large air pressure will be generated at the central axis of the wind guide chamber 109 suction power. The suction force can make the airborne material in the vicinity of the sampled target 133 be sucked into the vicinity of the center of the wind axis of the air guide chamber 109 from around the front hole of the air guide chamber 109, and form a sample gas column, along the central axis of the tornado airflow 132 moves downward, and finally the sample reaches the semi-permeable membrane 111 for sampling. This process is similar to the phenomenon of tornado-like "dragon fetching water" in nature.
一方面，采集的样品经半透膜111进入底盖113的漏斗形的腔内，在预热的情况快速气化并与从底盖113的侧壁中的载气通道121进来的载气气流137充分混合，之后载气携带样品进入进样接口120。On the one hand, the collected sample enters the funnel-shaped cavity of the bottom cover 113 through the semi-permeable membrane 111, and is quickly vaporized under the condition of preheating and flows with the carrier gas flowing in from the carrier gas channel 121 in the side wall of the bottom cover 113. 137 is fully mixed, and then the carrier gas carries the sample into the sampling interface 120.
另一方面，对于龙卷风式气流131的旋转中心的外围的气体，在龙卷风式气流131外围形成气旋沿导风腔109侧壁运动，在导风腔底部时，外围气旋的气体进入出口110，这部分气体形成旋风出气流134经排风口127排出。出口110设置成朝向气旋的气流方向，在图2中 示出的方位中，出口110可以斜向上，并且出口可以不是朝向腔体中心而是偏向内壁的切线方向，以便出口的开口方向更接近地朝向气流在出口处的速度方向。也就是说，虽然出口110的开口方向并没有严格与气流在出口处的速度方向相反，但是出口110的开口方向接近气流在出口处的速度方向的反向，以便气体更容易地进入出口110中被排出。On the other hand, for the gas on the periphery of the center of rotation of the tornado airflow 131, a cyclone is formed at the periphery of the tornado airflow 131 and moves along the sidewall of the wind guide chamber 109. When at the bottom of the wind guide chamber, the gas of the peripheral cyclone enters the outlet 110, which Part of the gas forms the cyclone outlet airflow 134 and is discharged through the exhaust port 127 . The outlet 110 is arranged to face the air flow direction of the cyclone. In the orientation shown in Fig. 2, the outlet 110 can be obliquely upward, and the outlet can be not toward the center of the cavity but the tangential direction of the inner wall, so that the opening direction of the outlet is closer to In the direction of the velocity of the airflow at the outlet. That is to say, although the opening direction of the outlet 110 is not strictly opposite to the velocity direction of the airflow at the outlet, the opening direction of the outlet 110 is close to the opposite direction of the velocity of the airflow at the outlet, so that the gas can enter the outlet 110 more easily was discharged.
通过这个过程，采样装置100持续地抽吸样品分子，如此实现对气载物质的放大采集。Through this process, the sampling device 100 continuously sucks the sample molecules, thus achieving amplified collection of airborne substances.
这种具有气体放大收集功能的龙卷风式实时采样装置100可直接用作IMS，GC，MS，GC-IMS，GC-MS等分析仪器的进样器，在此不再赘述。The tornado-type real-time sampling device 100 with the function of gas amplification and collection can be directly used as a sample injector for analytical instruments such as IMS, GC, MS, GC-IMS, and GC-MS, and will not be repeated here.
下面说明书根据本实用新型的采样装置的另一实施例。本实施例与以上所述的实施例类似，为了清楚下面仅描述其中不同的部分。Another embodiment of the sampling device according to the present invention will be described below. This embodiment is similar to the above-mentioned embodiments, and only the different parts are described below for clarity.
在根据本实用新型的实施例中，采样装置100包括第一端和与第一端相对的第二端。采样装置100包括腔体109，腔体的一部分105为漏斗形或截头圆锥形。具体地，腔体包括位于第一端附近的吸入样品的采样入口和位于第二端附近的排出样品的样品出口120。腔体109的采样入口位于截头圆锥形的内壁109的较小直径的圆形端部附近，并且截头圆锥形的内壁的较大直径圆形端部较靠近样品出口。In an embodiment according to the present invention, the sampling device 100 includes a first end and a second end opposite to the first end. Sampling device 100 includes a cavity 109, a portion 105 of which is funnel-shaped or frusto-conical. Specifically, the cavity includes a sampling inlet near the first end for sucking in the sample and a sample outlet 120 near the second end for discharging the sample. The sample inlet of the cavity 109 is located near the smaller diameter circular end of the frustoconical inner wall 109 and the larger diameter circular end of the frustoconical inner wall is closer to the sample outlet.
换句话说，漏斗形内壁109的小口径端用于对着样品，而大口径端朝向排出样品的样品出口。值得注意的是，在图中示出的腔体的方位是采样入口在上，排出样品的样品出口在下，因而漏斗形内壁109是倒置的漏斗布置形式。然而，这只是一种示例，当采样装置100水平放置对着被检测物体时，例如采样入口对着位于采样装置100左边的被检测物体时，漏斗形内壁109的小口一侧对着左侧被检测物体，此时漏斗形内壁109是横置的布置形式。In other words, the small-bore end of the funnel-shaped inner wall 109 is intended to face the sample, while the large-bore end faces toward the sample outlet from which the sample is discharged. It is worth noting that the orientation of the cavity shown in the figure is that the sampling inlet is on the top, and the sample outlet for discharging samples is on the bottom, so the funnel-shaped inner wall 109 is an inverted funnel arrangement. However, this is only an example. When the sampling device 100 is placed horizontally against the object to be detected, for example, when the sampling inlet is facing the object to be detected on the left side of the sampling device 100, the side of the small opening of the funnel-shaped inner wall 109 is placed against the left side. Detecting objects, at this time, the funnel-shaped inner wall 109 is arranged horizontally.
腔体还设有充气入口106，充气入口106配置成向腔体内吹入气流以便在腔体内产生龙卷风式气流。腔体还设有排气口110，排气口配置成排出气体以便与充气入口106一起在腔体内形成龙卷风式气流。具体地，充气入口106配置成使得充气入口106的轴向进气方向 沿与腔体内壁的内表面接近相切，并且充气入口106的轴向进气方向朝向样品出口倾斜，如图3示意地示出的图2中的沿A-A线的横截面。The cavity is also provided with an air inlet 106 configured to blow air into the cavity so as to generate a tornado-like air flow in the cavity. The cavity is also provided with an exhaust port 110 configured to exhaust gas so as to form a tornado-like flow of air within the cavity with the plenum inlet 106 . Specifically, the gas inlet 106 is configured such that the axial inlet direction of the gas inlet 106 is approximately tangent to the inner surface of the inner wall of the cavity, and the axial gas inlet direction of the gas inlet 106 is inclined toward the sample outlet, as shown schematically in FIG. 3 A cross-section along line A-A in Fig. 2 is shown.
在本实施例中可以不单独设置气帘引导体105，然而，通过在腔体内壁的靠近样品入口附近设置如上所述的充气入口106以及相应的进气通道也可以实现与上述气帘引导体105类似的效果。进一步，可以在腔体内部中形成如上述实施例中描述的气帘引导体的环形空间，环形空间配置成容纳气体以在环形空间内形成气压，并通过充气入口向采样装置100的内部空间充入气体。In this embodiment, the air curtain guide body 105 may not be provided separately, however, by arranging the above-mentioned inflation inlet 106 and the corresponding air inlet channel near the sample inlet on the inner wall of the cavity, it can also realize the similarity to the above air curtain guide body 105. Effect. Further, an annular space of the air curtain guide body as described in the above embodiments may be formed inside the cavity, the annular space is configured to accommodate gas to form an air pressure in the annular space, and fill the inner space of the sampling device 100 through the gas inlet. gas.
排气口110位于腔体的壁内，其设置形式可以与本实用新型的前面的实施例中的排气口类似，排气口110对着来自充气入口106的龙卷风式的螺旋前进的气流，使得气流尽可能地在较小阻力下进入排气口110。排气口110排出在腔体内形成的龙卷风式气流的外围气体。外围气体并不限定为空气，其中可能含有少量的样品。排气口的开口方向接近排气口处的气流的速度方向的反向。Exhaust port 110 is positioned at the wall of cavity, and its setting form can be similar to the vent port in the preceding embodiment of the present utility model, and exhaust port 110 faces the airflow that advances from the tornado type spiral of inflation inlet 106, The airflow is made to enter the exhaust port 110 with as little resistance as possible. The exhaust port 110 exhausts the peripheral air of the tornado airflow formed in the cavity. The ambient gas is not limited to air, which may contain a small amount of sample. The opening direction of the exhaust port is close to the opposite direction of the velocity of the airflow at the exhaust port.
采样装置100可以还包括位于采样入口一侧的第一端的过滤网，过滤网用于阻挡大颗粒物质进入采样入口，所述过滤网包括具有刚性的过滤大颗粒的粗滤网和过滤微颗粒的细滤网。The sampling device 100 may further include a filter screen located at the first end of the sampling inlet side, the filter screen is used to block large particles from entering the sampling inlet, and the filter screen includes a rigid coarse filter screen for filtering large particles and a filter screen for fine particles fine mesh.
采样装置100可以还包括用于控制腔体内温度的控温系统，包括设置在腔体的壁内的用于升温的加热器和用于测量温度的温度传感器。采样装置100可以还包括包围腔体的壁的保温层。在本实施例中腔体可以是一体形成的腔体，也可以是通过例如焊接、铆接等方式将多个部件接合在一起形成的腔体，对于本实用新型的技术方案这些形成方式并不对腔体内部的气流产生实质的影响。The sampling device 100 may further include a temperature control system for controlling the temperature in the cavity, including a heater for raising the temperature and a temperature sensor for measuring the temperature disposed in the wall of the cavity. The sampling device 100 may further include an insulating layer surrounding the walls of the cavity. In this embodiment, the cavity can be an integrally formed cavity, or it can be a cavity formed by joining multiple parts together by welding, riveting, etc. For the technical solution of the utility model, these formation methods are not suitable for the cavity have a substantial effect on the airflow inside the body.
本实施例中的腔体也可以设置与以上实施例相同的例如端盖101、滤网103、104、充气和排气气泵128、进样半透膜111、温控系统、保温层等。本实施例中的腔体还可以包括用于载气和样品混合的混合区。即，在腔体的下部，腔体具有混合区，混合区与腔体用于形成龙卷风式气流的部分隔开，例如可以使用半透膜111进行隔离。根据本实施例，可以设置两片网状金属112，以便对半透膜111进行 夹持保护，使半透膜112免受气流冲破。腔体的下部113可以包括载气通道121，用于注入载气，进来的载气在漏斗中与样品充分混合。腔体的下部113还可以包括进样口120，采集的样品与载气例如在混合预热后通过进样口120排出。类似地，腔体的底端面可以与本实用新型前面的实施例相同，如图4所示。腔体的底端面包括充气泵接口122、排气泵接口123、GC柱/离子迁移管接口124、加热棒引出线25、温度传感器引出线126、排风口127以及载气管接口136。充气泵接口122和排气泵接口123可以分别接一个气泵128，例如充气泵和排气泵，用于持续提供气体压力以便在采样装置100内部形成龙卷风式气流，其中排气泵流速是充气泵的10倍或更高。排气泵接口123期望布置成使得气阻尽可能小，因而排气泵接口在导风腔内的开口期望迎着气流的方向，使得气流容易地流入排气泵接口。排气泵接口123也可以不接气泵128直接用作排风口。为了使龙卷风式吸引放大的气流排出，可以多设计几个排风口127。GC柱/离子迁移管接口124可以接GC柱也可以直接接离子迁移管。载气管接口136接分子筛135以便使得载气得到净化。The cavity in this embodiment can also be provided with the same end caps 101, filter screens 103, 104, inflation and exhaust air pumps 128, sampling semi-permeable membrane 111, temperature control system, insulation layer, etc. as in the above embodiments. The chamber in this embodiment may also include a mixing zone for mixing of carrier gas and sample. That is, in the lower part of the cavity, the cavity has a mixing zone, which is separated from the part of the cavity for forming a tornado airflow, for example, by using a semi-permeable membrane 111 for isolation. According to this embodiment, two pieces of mesh metal 112 can be set, so that the semi-permeable membrane 111 is clamped and protected, and the semi-permeable membrane 112 is prevented from being broken by the airflow. The lower part 113 of the cavity may include a carrier gas channel 121 for injecting carrier gas, and the incoming carrier gas is fully mixed with the sample in the funnel. The lower part 113 of the chamber may also include a sample inlet 120 through which the collected sample and carrier gas are discharged through the sample inlet 120 after being mixed and preheated, for example. Similarly, the bottom surface of the cavity can be the same as the previous embodiment of the present invention, as shown in FIG. 4 . The bottom surface of the cavity includes an air pump interface 122, an exhaust pump interface 123, a GC column/ion transfer tube interface 124, a heating rod lead line 25, a temperature sensor lead line 126, an exhaust port 127 and a carrier gas tube interface 136. The air pump interface 122 and the exhaust pump interface 123 can be respectively connected with an air pump 128, such as an air pump and an exhaust pump, for continuously providing gas pressure so as to form a tornado-style airflow inside the sampling device 100, wherein the flow rate of the exhaust pump is 10 times that of the air pump or higher. The exhaust pump interface 123 is expected to be arranged so that the air resistance is as small as possible, so the opening of the exhaust pump interface in the air guide chamber is expected to face the direction of the airflow, so that the airflow can easily flow into the exhaust pump interface. The exhaust pump interface 123 can also be directly used as an air exhaust port without connecting the air pump 128 . In order to make the airflow amplified by the tornado-like suction exhaust, several more air outlets 127 can be designed. The GC column/ion transfer tube interface 124 can be connected to the GC column or directly connected to the ion transfer tube. The carrier gas pipe interface 136 is connected to a molecular sieve 135 to purify the carrier gas.
此外，根据本实用新型的采样装置的又一实施例，本实用新型中的腔体的一部分的截头圆锥形内壁可以不是严格的截头圆锥形，而可以是球形的一部分。也就是说，腔体的一部分的内壁是弧面，只要样品进入一侧的腔体内壁的直径较小，排出样品一侧的腔体内壁直径较大以便在腔体内部形成龙卷风式气流即可。In addition, according to yet another embodiment of the sampling device of the present invention, the frusto-conical inner wall of a part of the cavity in the present invention may not be strictly frusto-conical, but may be a part of a sphere. That is to say, the inner wall of a part of the cavity is an arc surface, as long as the diameter of the inner wall of the cavity on the side where the sample enters is smaller, and the diameter of the inner wall of the cavity on the side where the sample is discharged is larger to form a tornado-like airflow inside the cavity .
根据本实用新型的检测设备的另一实施例，检测设备的预处理进样装置的一个实施例在图5中更详细地示意地示出。According to another embodiment of the detection device of the present invention, an embodiment of the pretreatment sampling device of the detection device is schematically shown in more detail in FIG. 5 .
如图4所示，预处理进样装置主要包括活塞式吸附器202、活塞缸203、热解析腔204和泵205。以下将详细各个部件的结构和操作。As shown in FIG. 4 , the pretreatment sampling device mainly includes a piston adsorber 202 , a piston cylinder 203 , a thermal analysis chamber 204 and a pump 205 . The structure and operation of each component will be described in detail below.
采样装置100通过连接管与活塞缸203连接并连通。The sampling device 100 is connected and communicated with the piston cylinder 203 through a connecting pipe.
连接管内可以放置有干燥剂，干燥剂可以吸收样品采集过程中混在所采集的样品中的水分、湿气等，能够起到保护分析仪器的色谱柱、迁移管的作用。干燥剂可以被包在干燥剂包中，在连接管内可以设置用于固定干燥剂或干燥剂包的结构，如凸起，以防止干燥剂或干燥剂 包在泵的抽吸作用下移动。A desiccant can be placed in the connecting pipe, and the desiccant can absorb the moisture and moisture mixed in the sample collected during the sample collection process, and can protect the chromatographic column and the migration tube of the analytical instrument. The desiccant can be wrapped in a desiccant bag, and a structure for fixing the desiccant or the desiccant bag can be arranged in the connecting pipe, such as a protrusion, to prevent the desiccant or the desiccant bag from moving under the suction of the pump.
连接管的至少一个部分，如在干燥剂之后的部分，可以由可伸缩软管或波纹管构成，在取样时可以对这种可伸缩软管或波纹管可进行拉伸和/或旋转，从而调整样品采集口的方向，极大的方便了用户对样品的采集。连接管的末端被构造成密封地和可拆卸地连接至活塞缸203。At least one part of the connecting pipe, such as the part after the desiccant, can be formed by a telescopic hose or bellows, which can be stretched and/or rotated during sampling, so that Adjusting the direction of the sample collection port greatly facilitates the user to collect samples. The end of the connecting pipe is configured to be hermetically and detachably connected to the piston cylinder 203 .
图6示意性地示出了本实用新型一个实施例的预处理进样装置的活塞式吸附器的一个示例。如图所示，活塞式吸附器202整体上为一个可在活塞缸203内往复运动的柱形活塞形式，主要包括活塞杆体221和连接至活塞杆体221的末端的吸附腔222。活塞杆体221可以由化学性质稳定的耐热型材料(如聚四氟)制成。Fig. 6 schematically shows an example of a piston adsorber of a pretreatment sampling device according to an embodiment of the present invention. As shown in the figure, the piston-type adsorber 202 is generally in the form of a cylindrical piston that can reciprocate in the piston cylinder 203 , and mainly includes a piston rod body 221 and an adsorption chamber 222 connected to the end of the piston rod body 221 . The piston rod body 221 can be made of chemically stable heat-resistant material (such as polytetrafluoro).
在一个示例中，吸附腔222可以包括内部填充有吸附剂223的网状结构，即腔壁上开口有网状小孔，腔内部放置吸附剂。吸附剂材料的吸附特性可根据不同的检测需求进行选择性添加，这种按需选择方式，在一定程度上增强了对检测样品的选择性吸附。可以理解，所填充的吸附剂的直径应大于网状结构的网孔孔径。如图6所示，吸附腔222可以具有部分中空形式，即可以包括吸附通道226，其可以为L形或拐杖形，在腔壁上具有开口。如下文将描述的那样，该吸附通道在采样时与样品采集结构连通，以接收经由连接管被抽吸进近来的样品。这样，不仅能方便样品进入吸附剂，而且能增大样品与吸附剂的接触面积，有利于样品吸附。In one example, the adsorption chamber 222 may include a mesh structure filled with an adsorbent 223 inside, that is, a mesh-like hole is opened on the wall of the chamber, and the adsorbent is placed inside the chamber. The adsorption characteristics of the adsorbent material can be selectively added according to different detection requirements. This on-demand selection method enhances the selective adsorption of the detection sample to a certain extent. It can be understood that the diameter of the filled adsorbent should be larger than the mesh pore diameter of the network structure. As shown in FIG. 6 , the adsorption chamber 222 may have a partially hollow form, that is, may include an adsorption channel 226 , which may be L-shaped or crutch-shaped, with an opening on the chamber wall. As will be described below, the adsorption channel communicates with the sample collection structure during sampling, so as to receive the sample sucked in through the connecting tube. In this way, it is not only convenient for the sample to enter the adsorbent, but also increases the contact area between the sample and the adsorbent, which is beneficial to the adsorption of the sample.
在一个示例中，活塞杆体221可以包括冷却通道227和形成在活塞杆体的下部中的多个通孔228。如下文所述，冷却通道227被构造成在活塞式吸附器位于样品采集位置中时直接与环境气体连通，并在活塞式吸附器位于样品解析位置中时通过形成在活塞缸中的冷却通孔与环境气体连通。冷却通道227也可以是L形或拐杖形，具有通向环境气体的开口；通孔228被构造成能够与冷却通道227和活塞缸203的内部连通。这种中空的活塞杆体一方面能够减小活塞式吸附器的质量，有利于吸附器快速升、降温，另一方面在解析进样时还可将泵205与活塞缸203的上部的冷却气入口235(参见图5和图7)连通， 采用泵抽气可对吸附器上部进行风冷，加快了活塞式吸附器上部的降温速度，有助于位于活塞式吸附器下半部分的吸附腔及腔内的吸附剂的快速降温，进而有利于样品吸附。In one example, the piston rod body 221 may include a cooling passage 227 and a plurality of through holes 228 formed in a lower portion of the piston rod body. As described below, the cooling channel 227 is configured to communicate directly with the ambient gas when the piston adsorber is in the sample collection position, and through cooling vias formed in the piston cylinder when the piston adsorber is in the sample analysis position In communication with ambient gas. The cooling channel 227 can also be L-shaped or crutch-shaped, with an opening leading to ambient air; the through hole 228 is configured to be able to communicate with the cooling channel 227 and the interior of the piston cylinder 203 . On the one hand, this hollow piston rod can reduce the mass of the piston-type adsorber, which is beneficial to the rapid rise and fall of the adsorber. 235 (see Fig. 5 and Fig. 7), the upper part of the adsorber can be air-cooled by pumping air, which speeds up the cooling rate of the upper part of the piston-type adsorber, and is helpful for the adsorption chamber located in the lower part of the piston-type adsorber and The rapid cooling of the adsorbent in the chamber facilitates the adsorption of samples.
根据本实用新型的一个实施例，活塞式吸附器202还可以包括可拆卸地连接至吸附腔222的远离活塞杆体221的一端的隔热垫224，即吸附腔222位于活塞杆体221和隔热垫224之间。示例性地，通过拔出活塞式吸附器或拧下活塞缸，并旋开或去除位于吸附器底部的隔热垫，可以更换吸附腔内的吸附剂。隔热垫可以由聚四氟材料制成，隔热垫的设置能够减少热解析腔至吸附腔的热传递，能有效地保证在活塞式吸附器进行采样/富集时吸附腔和吸附剂保持低温，如处于近乎室温，有利于样品吸附和富集。According to an embodiment of the present utility model, the piston-type adsorber 202 can also include a heat insulation pad 224 detachably connected to the end of the adsorption chamber 222 away from the piston rod body 221, that is, the adsorption chamber 222 is located between the piston rod body 221 and the heat insulation pad. Between 224. Exemplarily, the adsorbent in the adsorption chamber can be replaced by pulling out the piston type adsorber or unscrewing the piston cylinder, and unscrewing or removing the heat insulation pad at the bottom of the adsorber. The heat insulation pad can be made of PTFE material. The setting of the heat insulation pad can reduce the heat transfer from the pyrolysis chamber to the adsorption chamber, and can effectively ensure that the adsorption chamber and the adsorbent remain stable when the piston adsorber performs sampling/enrichment. Low temperature, such as near room temperature, is conducive to sample adsorption and enrichment.
在一个实施例中，多个密封圈225套设在活塞式吸附器202上，如在活塞式吸附器202的外表面上，使得活塞式吸附器202能够被密封地容纳在活塞缸203内。优选地，密封圈225的布置使得在活塞式吸附器202在活塞缸203内的最高位置(如样品采集位置)和最低位置(如样品解析位置)之间往复移动时，活塞式吸附器202都能够通过密封圈225与活塞缸203的内壁保持密封接触，如图5和7所示。示例性地，在吸附通道226的开口上下的位置处、以及冷却通道227的开口的上下位置处，都设置有密封圈225，如图6所示。In one embodiment, a plurality of sealing rings 225 are sleeved on the piston adsorber 202 , such as on the outer surface of the piston adsorber 202 , so that the piston adsorber 202 can be hermetically accommodated in the piston cylinder 203 . Preferably, the arrangement of the sealing ring 225 is such that when the piston-type adsorber 202 reciprocates between the highest position (such as a sample collection position) and the lowest position (such as a sample analysis position) in the piston cylinder 203, the piston-type adsorber 202 is It can be kept in sealing contact with the inner wall of the piston cylinder 203 through the sealing ring 225 , as shown in FIGS. 5 and 7 . Exemplarily, sealing rings 225 are provided at positions above and below the opening of the adsorption channel 226 and at positions above and below the opening of the cooling channel 227 , as shown in FIG. 6 .
活塞式吸附器202的活塞杆体221的末端还可以设置有推拉手柄229，推拉手柄229用于由用户推拉活塞式吸附器202在活塞缸203内往复运动。The end of the piston rod body 221 of the piston-type adsorber 202 can also be provided with a push-pull handle 229 , and the push-pull handle 229 is used for pushing and pulling the piston-type adsorber 202 to reciprocate in the piston cylinder 203 .
如图5和7所示，活塞缸203主要包括缸体231和用于容纳活塞式吸附器202并与吸附腔222连通的活塞腔232。缸体231可以由强度大、耐热好、化学性质稳定的聚四氟材料制成，并限定活塞腔232的至少一部分。缸体231安装在热解析腔204上，缸体231上设置有与活塞腔232连通的采样连接气嘴233。如上所述，采样装置100的连接管末端可以密封地和可拆卸地安装或插接在采样连接气嘴233中，从而实现采样装置100的内部样品通道与活塞腔232的连通。采样连接气嘴233中可以设置有控制这种连通的开启和关闭的阀。As shown in FIGS. 5 and 7 , the piston cylinder 203 mainly includes a cylinder body 231 and a piston chamber 232 for accommodating the piston adsorber 202 and communicating with the adsorption chamber 222 . The cylinder body 231 can be made of polytetrafluoro material with high strength, good heat resistance and stable chemical properties, and defines at least a part of the piston cavity 232 . The cylinder body 231 is installed on the thermal analysis chamber 204 , and the cylinder body 231 is provided with a sampling connection gas nozzle 233 communicating with the piston cavity 232 . As mentioned above, the end of the connecting tube of the sampling device 100 can be hermetically and detachably installed or plugged into the sampling connection nozzle 233 , so as to realize the communication between the internal sample channel of the sampling device 100 and the piston chamber 232 . A valve that controls the opening and closing of this communication may be provided in the sampling connection gas nozzle 233 .
缸体231还设置有泵连接气嘴234，泵205通过导管251连接至气嘴234进而与活塞腔232连通，以便在样品采样/富集或预浓缩时，泵205、导管251、泵连接气嘴234、活塞腔232、采样连接气嘴233、连接管样品采集口构成连通通路，开启泵205可以将环境气体中的待采样的样品(如，挥发性、半挥发性物质或表面沾染物质)抽取到吸附腔222中，由吸附腔222吸附/预浓缩。在样品采样期间，泵205持续工作，可以在吸附腔内富集或预浓缩样品。采样过程中整个活塞式吸附器处于室温。The cylinder body 231 is also provided with a pump connection gas nozzle 234, and the pump 205 is connected to the gas nozzle 234 through a conduit 251 and then communicated with the piston chamber 232, so that when the sample is sampled/enriched or pre-concentrated, the pump 205, the conduit 251, and the pump connection gas Nozzle 234, piston chamber 232, sampling connection gas nozzle 233, and connection tube sample collection port constitute a communication path, and the sample to be sampled (such as volatile, semi-volatile substances or surface contamination substances) in the ambient gas can be turned on by opening the pump 205 It is pumped into the adsorption chamber 222, and is adsorbed/pre-concentrated by the adsorption chamber 222. During sample sampling, the pump 205 works continuously to enrich or pre-concentrate the sample in the adsorption chamber. The entire piston adsorber was at room temperature during the sampling process.
活塞缸203还可以包括设置在热解析腔204内以引导活塞式吸附器202在热解析腔202内的运动的导轨236，其能有效防止活塞式吸附器202晃动，增强牢固程度。导轨236连接至缸体231，并限定活塞腔232的一部分。The piston cylinder 203 may also include a guide rail 236 arranged in the thermal analysis chamber 204 to guide the movement of the piston adsorber 202 in the thermal analysis chamber 202, which can effectively prevent the piston adsorber 202 from shaking and enhance its firmness. The rail 236 is connected to the cylinder 231 and defines a portion of the piston chamber 232 .
如图5和7所示，热解析腔204主要包括腔体241和由腔体241限定的用于对样品进行热解析的内部空间。在腔体241上设置有载气入口242、分流和/或吹扫出气口243、和用于连接诸如色谱柱或IMS之类的分析仪器的接口244。As shown in FIGS. 5 and 7 , the thermal analysis chamber 204 mainly includes a cavity 241 and an inner space defined by the cavity 241 for performing thermal analysis on samples. The cavity 241 is provided with a carrier gas inlet 242 , a split flow and/or purge outlet 243 , and an interface 244 for connecting to an analytical instrument such as a chromatographic column or IMS.
在热解析腔204的腔体内，可以密封植入化学性质稳定的衬管245，其能有效避免样品与热解析腔的金属壁的直接接触。衬管245可定期更换，防止样品对热解析腔的直接污染，降低了样品失真率，提高了样品检测精度及可靠度。在热解析腔204的腔体外壁可以包覆有加热结构或加热膜，用于给热解析腔204加热。热解析腔204可以设置有温度传感器，如在腔体外表面上，用于实时检测和监测热解析腔内的温度。此外，在热解析腔204的腔体外壁还可以包覆有保温棉，用于给热解析腔保温，以便节省能耗。加热结构、温度传感器和/或保温棉构成热解析温控系统的部件，用于在控制器的控制下将热解析腔的温度维持在一恒定高温处，如80℃～300℃。热解析腔可以采用程序升温模式，可以减小功率消耗。In the cavity of the thermal analysis chamber 204, a chemically stable liner 245 can be hermetically implanted, which can effectively avoid direct contact between the sample and the metal wall of the thermal analysis chamber. The liner 245 can be replaced regularly to prevent the sample from directly polluting the thermal analysis chamber, reduce the sample distortion rate, and improve the detection accuracy and reliability of the sample. The outer wall of the thermal analysis chamber 204 may be coated with a heating structure or a heating film for heating the thermal analysis chamber 204 . The thermal desorption chamber 204 may be provided with a temperature sensor, such as on the outer surface of the chamber, for real-time detection and monitoring of the temperature in the thermal desorption chamber. In addition, the outer wall of the thermal analysis chamber 204 may also be covered with thermal insulation cotton, which is used to keep the thermal analysis chamber warm, so as to save energy consumption. The heating structure, temperature sensor and/or thermal insulation cotton constitute the components of the thermal desorption temperature control system, which are used to maintain the temperature of the thermal desorption chamber at a constant high temperature under the control of the controller, such as 80°C-300°C. The thermal analysis chamber can adopt temperature programming mode, which can reduce power consumption.
在热解析腔204和活塞缸203之间还可以设置或插入隔热结构，如多孔陶瓷绝热盘，其能在样品解析期间有效地隔绝热解析腔与活塞式吸附器的上半部分(如活塞杆体)之间的热交换，在样品采集期间有 效地隔绝热解析腔与活塞式吸附器之间的热交换，以及有效地隔绝热解析腔与活塞缸上半部分之间的热交换，确保了样品采集过程中整个活塞式吸附器均处于室温，有利于样品的采集。Between the thermal analysis chamber 204 and the piston cylinder 203, a thermal insulation structure can also be set or inserted, such as a porous ceramic heat insulating plate, which can effectively isolate the thermal analysis chamber from the upper half of the piston type adsorber (such as the piston) during sample analysis. The heat exchange between the rod body), effectively insulate the heat exchange between the thermal analysis chamber and the piston-type adsorber during sample collection, and effectively isolate the heat exchange between the thermal analysis chamber and the upper half of the piston cylinder, to ensure This ensures that the entire piston adsorber is at room temperature during the sample collection process, which is beneficial to sample collection.
在需要对样品进行热解析进样时，先启动热解析温控系统将热解析腔的温度维持在一个合适的恒定高温(80℃～300℃)，将吸附有样品的活塞式吸附器快速推至具有高温的热解析腔内，被推入热解吸腔中的吸附剂被迅速加热，吸附腔内吸附的样品在高温下瞬间析出，析出的样品与从热解析腔的载气入口引入的经预热的载气混合，最终被载气带入检测器或分析仪器中进行检测或分析。When it is necessary to inject the sample by thermal analysis, first start the thermal analysis temperature control system to maintain the temperature of the thermal analysis chamber at a suitable constant high temperature (80 ° C ~ 300 ° C), and quickly push the piston adsorber with the sample adsorbed. Into the thermal analysis chamber with high temperature, the adsorbent pushed into the thermal desorption chamber is heated rapidly, and the sample adsorbed in the adsorption chamber is precipitated at high temperature instantly, and the precipitated sample is combined with the carrier gas introduced from the thermal analysis chamber. The preheated carrier gas is mixed and finally brought into the detector or analysis instrument by the carrier gas for detection or analysis.
如上所述，在将吸附腔推至热解析腔内的同时，泵205、活塞腔232、形成在活塞杆体中的多个通孔228、冷却通道227、和活塞缸203上的冷却气入口235形成连通通路，因此，可采用泵205抽气对留在热解析腔外的活塞式吸附器的上半部分(包括活塞杆体)进行风冷，有利于下一次的样品吸附和富集或预浓缩。As mentioned above, while pushing the adsorption chamber into the thermal desorption chamber, the pump 205, the piston chamber 232, the plurality of through holes 228 formed in the piston rod body, the cooling channel 227, and the cooling air inlet 235 on the piston cylinder 203 A communication path is formed, therefore, the upper half of the piston adsorber (including the piston rod body) left outside the thermal analysis chamber can be air-cooled by pumping air through the pump 205, which is beneficial to the next sample adsorption and enrichment or pre-concentration .
这种具有富集或预浓缩功能的预处理进样装置可直接用作IMS谱仪或GC，也可用作IMS-GC，GC-MS等痕量化学物质分析谱仪的进样器，在此不再赘述。This pretreatment sampling device with enrichment or preconcentration function can be directly used as an IMS spectrometer or GC, and can also be used as a sampler for IMS-GC, GC-MS and other trace chemical substance analysis spectrometers. This will not be repeated here.
以下将参照图5和7描述上述预处理进样装置的操作。首先，拉动并定位活塞式吸附器202在如图5所示的样品采集位置中，使得吸附腔222与采样装置100连通，此时，泵205、导管251、泵连接气嘴234、活塞腔232的一部分(包括围绕吸附腔的部分)、采样连接气嘴233、连接管和样品采集口124借助于密封圈225构成连通通路，随后，启动泵205工作，以将环境气体中的待采样的样品(如，挥发性、半挥发性物质或表面沾染物质)抽取到吸附腔222中，由吸附腔222吸附/预浓缩。在样品采样期间，泵205可以持续工作，以在吸附腔内富集或预浓缩样品。采样过程中整个活塞式吸附器处于室温。The operation of the above-mentioned pretreatment sampling device will be described below with reference to FIGS. 5 and 7 . First, pull and position the piston-type adsorber 202 in the sample collection position as shown in FIG. A part (including the part surrounding the adsorption chamber), the sampling connection gas nozzle 233, the connecting pipe and the sample collection port 124 form a communication path by means of the sealing ring 225, and then the pump 205 is started to work, so that the sample to be sampled in the ambient gas (eg, volatile, semi-volatile substances or surface contamination substances) are drawn into the adsorption chamber 222, and are adsorbed/pre-concentrated by the adsorption chamber 222. During sample sampling, the pump 205 can work continuously to enrich or pre-concentrate the sample in the adsorption chamber. The entire piston adsorber was at room temperature during the sampling process.
接着，启动热解析温控系统以将热解析腔204的温度维持在一恒定高温处，然后快速移动并将活塞式吸附器202定位在如图7所示的样品解析位置中，使得吸附腔222定位在热解析腔204内。吸附腔222可以通过密封圈225被密封在活塞腔232的下部中并进而被密封 在热解析腔204内。此时，被推入热解吸腔204中的吸附剂被迅速加热，吸附腔222内吸附的样品在高温下瞬间析出，析出的样品与从热解析腔204的载气入口242引入的经预热的载气混合，最终被载气带入检测器或分析仪器(未示出)中进行检测或分析。Then, start the thermal analysis temperature control system to maintain the temperature of the thermal analysis chamber 204 at a constant high temperature, then quickly move and position the piston adsorber 202 in the sample analysis position as shown in Figure 7, so that the adsorption chamber 222 Positioned within the thermal desorption chamber 204 . Adsorption chamber 222 can be sealed in the lower part of piston chamber 232 by sealing ring 225 and then be sealed in thermal analysis chamber 204. At this time, the adsorbent pushed into the thermal desorption chamber 204 is rapidly heated, and the sample adsorbed in the adsorption chamber 222 is precipitated at high temperature instantaneously. The hot carrier gas mixes and is eventually carried by the carrier gas to a detector or analytical instrument (not shown) for detection or analysis.
在样品在热解析腔内的解析期间，泵205、导管251、泵连接气嘴234、活塞腔232的一部分(即在热解析腔204之外的部分)、形成在活塞杆体221中的多个通孔228、冷却通道227、和活塞缸203上的冷却气入口235形成与环境气体连通的通路或空间。因此，可采用泵205抽气对留在热解析腔204外的活塞式吸附器202的上半部分(包括活塞杆体)进行风冷，从而能够将活塞式吸附器的定位在热解析腔外的部分保持在室温，有利于下一次的样品吸附和富集或预浓缩。During the analysis of the sample in the thermal analysis chamber, the pump 205, the conduit 251, the pump connection gas nozzle 234, a part of the piston chamber 232 (that is, the part outside the thermal analysis chamber 204), a plurality of valves formed in the piston rod body 221 The through hole 228, the cooling passage 227, and the cooling gas inlet 235 on the piston cylinder 203 form a passage or space that communicates with the ambient gas. Therefore, pump 205 can be used to air-cool the upper half (including the piston rod) of the piston adsorber 202 outside the thermal analysis chamber 204, so that the piston adsorber can be positioned outside the thermal analysis chamber. Partially kept at room temperature is conducive to the next sample adsorption and enrichment or pre-concentration.
参照图8，示出本实用新型的检测设备的另一实施例的预处理进样装置300。预处理进样装置300包括：吸气泵320、吸附器330、活塞缸体340和解析缸体350。解析缸体350具有解析腔356，解析缸体350设有与解析腔356连通的分析仪器接口352、载气入口351和载气分流/吹扫接口353，解析缸体350的外壁设有加热膜及温度传感器(图未示出)。分析仪器接口用于与色谱柱、IMS、MS或DMS等连接；载气入口与载气供给装置连接，用于接收载气；加热膜用于加热解析腔356，温度传感器用于实时读取解析腔温度并和外部温控电路连接以实现对温度的控制。活塞缸体340设有两个活塞腔341，每个活塞腔341安装一个吸附器330。活塞缸体340安装在解析缸体350上，且两个活塞腔341均与解析腔356相连通。活塞缸体340的下部伸入解析腔356中，活塞腔341的前部为开口，与解析腔356相连通。活塞缸体340设有均与两个活塞腔341连通的样品进气口342和吸气泵气口343，样品进气口342与采样器100通过波纹软管312连接，吸气泵气口343与吸气泵320连接。吸附器330包括相连接的吸附筛筒332和活塞杆331。吸附筛筒332为一个侧壁设有细孔的圆筒，吸附筛筒332用于存放吸附剂。吸附器330的整体结构呈一个可往复运动的圆柱形活塞。活塞杆331可滑动安装在活塞腔341中，带动吸附筛筒332沿活塞腔341滑动并可伸入解析腔356中，且吸附筛 筒332可同时与样品进气口342和吸气泵气口343连通。为了方便推拉活塞杆331，在活塞杆的后端设有一个活塞手柄371。Referring to FIG. 8 , it shows a pretreatment sampling device 300 of another embodiment of the detection device of the present invention. The pretreatment sampling device 300 includes: an air suction pump 320 , an adsorber 330 , a piston cylinder 340 and an analysis cylinder 350 . The analysis cylinder 350 has an analysis chamber 356, and the analysis cylinder 350 is provided with an analysis instrument interface 352 connected with the analysis chamber 356, a carrier gas inlet 351, and a carrier gas splitting/purging interface 353, and the outer wall of the analysis cylinder 350 is provided with a heating film and a temperature sensor (not shown). The analytical instrument interface is used to connect with chromatographic column, IMS, MS or DMS, etc.; the carrier gas inlet is connected to the carrier gas supply device to receive carrier gas; the heating film is used to heat the analysis chamber 356, and the temperature sensor is used to read and analyze in real time The cavity temperature is connected with the external temperature control circuit to realize the temperature control. The piston cylinder 340 is provided with two piston chambers 341 , and each piston chamber 341 is equipped with an adsorber 330 . The piston cylinder 340 is installed on the analysis cylinder 350 , and the two piston chambers 341 are both connected to the analysis chamber 356 . The lower part of the piston cylinder 340 extends into the analysis cavity 356 , and the front part of the piston cavity 341 is an opening, which communicates with the analysis cavity 356 . The piston cylinder 340 is provided with a sample air inlet 342 and an aspirator pump air port 343 that are both connected to the two piston chambers 341. The sample air inlet 342 is connected to the sampler 100 through a corrugated hose 312, and the aspirator pump air port 343 is connected to the air suction pump. Air pump 320 is connected. The adsorber 330 includes a connected adsorption screen cylinder 332 and a piston rod 331 . The adsorption sieve cylinder 332 is a cylinder with fine holes on the side wall, and the adsorption sieve cylinder 332 is used to store the adsorbent. The overall structure of the adsorber 330 is a reciprocating cylindrical piston. The piston rod 331 can be slidably installed in the piston chamber 341, and drives the adsorption sieve cylinder 332 to slide along the piston chamber 341 and can extend into the analysis chamber 356, and the adsorption sieve cylinder 332 can be connected with the sample inlet 342 and the suction pump inlet 343 at the same time. connected. In order to push and pull the piston rod 331 conveniently, a piston handle 371 is provided at the rear end of the piston rod.
在使用时，在吸附筛筒332中放置吸附剂，先将吸附器330拉起，使吸附筛筒332与采样器100及吸气泵320连通，吸气泵320吸气，采样器100吸收样品气，样品气流过吸附筛筒332，样品气中的样品被吸附剂吸收，待吸附剂上的样品量富集后，将吸附器330摁入已预先加热的解析腔356中进行样品析出，析出的样品在解析腔356中与经预热的从载气入口351流入解析腔内的载气均匀混合后从分析仪器接口352进入GC-IMS、IMS、GC-MS、GC-DMS或其它分析仪器中，进行检测。本实用新型的两个吸附器330可以交替使用，即一个拉起时取样时(后一被检样品)，另一个摁下进行样品解析和检测(前一被检样品)，使进样装置能够全时、快速地吸收样品，尤其是在处理有多个被检样品时体现出了明显的检测优越性。吸附器可对样品进行浓缩，提高了分析仪器的检测精确度。When in use, place an adsorbent in the adsorption sieve cylinder 332, first pull up the adsorber 330, make the adsorption sieve cylinder 332 communicate with the sampler 100 and the suction pump 320, the suction pump 320 inhales, and the sampler 100 absorbs the sample gas, the sample gas flows through the adsorption sieve cylinder 332, and the sample in the sample gas is absorbed by the adsorbent. After the sample amount on the adsorbent is enriched, the adsorber 330 is pressed into the pre-heated analysis chamber 356 for sample precipitation. The sample in the analysis chamber 356 is evenly mixed with the preheated carrier gas flowing into the analysis chamber from the carrier gas inlet 351, and then enters the GC-IMS, IMS, GC-MS, GC-DMS or other analysis instruments from the analysis instrument interface 352 , for detection. The two adsorbers 330 of the present utility model can be used alternately, that is, when one is pulled up to take a sample (the next tested sample), the other is pressed down to perform sample analysis and detection (the previous tested sample), so that the sampling device can It absorbs samples full-time and quickly, especially when dealing with multiple samples to be tested, it shows obvious detection advantages. The adsorber can concentrate the sample, which improves the detection accuracy of the analytical instrument.
根据一个实施例，吸附筛筒332设有一个吸附筛口372，吸附筛口372可与样品进气口342连通，样品气进入时，快速地从吸附筛口372进入吸附筛筒中，采用形如372的结构，有效的增大了单位时间内的吸附面积，提高样品富集的速度。优选的，样品进气口342和吸气泵气口343沿活塞腔341的轴向方向设置，样品进气口342和吸气泵气口343之间的距离略小于吸附筛筒332的长度，使吸附筛口372恰好能够与样品进气口342相对连通。同时，还可以通过旋开位于吸附器顶端的绝热垫333对吸附筛筒332中的吸附剂进行更换，吸附剂类型可按检测需求选择。According to one embodiment, the adsorption sieve 332 is provided with an adsorption sieve 372, the adsorption sieve 372 can communicate with the sample gas inlet 342, when the sample gas enters, it will quickly enter the adsorption sieve from the adsorption sieve 372. The structure of 372 effectively increases the adsorption area per unit time and improves the speed of sample enrichment. Preferably, the sample inlet 342 and the aspirator pump inlet 343 are arranged along the axial direction of the piston chamber 341, and the distance between the sample inlet 342 and the aspirator pump inlet 343 is slightly smaller than the length of the adsorption sieve cylinder 332, so that the adsorption The sieve opening 372 is just able to communicate with the sample inlet 342 oppositely. At the same time, the adsorbent in the adsorption screen cylinder 332 can also be replaced by unscrewing the heat insulating pad 333 located at the top of the adsorber, and the type of adsorbent can be selected according to the detection requirements.
根据一个实施例，解析缸体350的外壁还设有温度传感器(图未示出)和保温层354。温度传感器用于检测解析缸体的温度，同时，温度传感器与一个控制器连接，通过控制器以程序升温的形式控制解析腔356的温度，能有效的减小功率消耗。保温层351采用保温棉，用于给解析缸体保温，以降低能耗。解析缸体350还设有一个载气分流/吹扫接口353，载气分流口353与解析腔356相连通，分析仪器接口352无法完全接收混合样品气时，混合样品气从载气分流/吹扫口 排出。活塞缸体340与解析缸体350之间设有隔热盘360，能够有效地隔绝解析缸体350及活塞缸体340的热传递。活塞缸体340及解析缸体350与隔热盘360之间采用螺纹密封连接。隔热盘360采用多孔陶瓷材料制成。According to an embodiment, the outer wall of the analysis cylinder 350 is further provided with a temperature sensor (not shown in the figure) and a thermal insulation layer 354 . The temperature sensor is used to detect the temperature of the analysis cylinder, and at the same time, the temperature sensor is connected with a controller, and the temperature of the analysis chamber 356 is controlled by the controller in the form of temperature increase, which can effectively reduce power consumption. The thermal insulation layer 351 adopts thermal insulation cotton, which is used for thermal insulation of the analysis cylinder to reduce energy consumption. The analysis cylinder 350 is also provided with a carrier gas split/purge interface 353, the carrier gas split port 353 is connected with the analysis chamber 356, and when the analysis instrument interface 352 cannot completely receive the mixed sample gas, the mixed sample gas is split/purged from the carrier gas. Sweep out. A heat insulating plate 360 is provided between the piston cylinder 340 and the analysis cylinder 350 , which can effectively isolate the heat transfer between the analysis cylinder 350 and the piston cylinder 340 . The piston cylinder 340 , the analytical cylinder 350 and the heat shield 360 are connected by thread sealing. The thermal insulation plate 360 is made of porous ceramic material.
为了获取干燥的样品气，在波纹炊管312中设置干燥剂包313，用于除去混合气体中的水蒸气，起到保护色谱柱及检测器的作用。干燥剂包313通过设置在波纹软管312中卡槽314固定安装。采样器310具有一个喇叭吸气头311，喇叭吸气头311上设有微孔滤网315。在设置微孔滤网15，可防止大颗粒物质进入而堵塞管路。In order to obtain dry sample gas, a desiccant bag 313 is set in the corrugated cooking tube 312 to remove water vapor in the mixed gas and protect the chromatographic column and detector. The desiccant package 313 is fixedly installed through the slot 314 provided in the corrugated hose 312 . The sampler 310 has a horn suction head 311 , and a microporous filter 315 is arranged on the horn suction head 311 . When the microporous filter screen 15 is set, it can prevent large particles from entering and clogging the pipeline.
根据一个实施例，每个活塞腔341设有一个冷却气口344，冷却气口344设有入口阀门374。活塞杆331设有冷却空腔334，冷却空腔334可与冷却气口344连通，且活塞杆331的侧壁设有与冷却空腔334连接的多个通风孔373，至少部分通风孔373可与吸气泵气口连通。当需要对吸附器330冷却时，拉起吸附器330，使冷却空腔334与冷却气口344连接，打开入口阀门374，在吸气泵的作用下，冷却气从冷却气口344流入，对活塞杆331和吸附筛筒332进行冷却。According to one embodiment, each piston cavity 341 is provided with a cooling air port 344 , and the cooling air port 344 is provided with an inlet valve 374 . The piston rod 331 is provided with a cooling cavity 334, the cooling cavity 334 can communicate with the cooling air port 344, and the side wall of the piston rod 331 is provided with a plurality of ventilation holes 373 connected with the cooling cavity 334, at least part of the ventilation holes 373 can be connected with the cooling cavity 334. The gas port of the suction pump is connected. When the adsorber 330 needs to be cooled, the adsorber 330 is pulled up, the cooling cavity 334 is connected to the cooling air port 344, the inlet valve 374 is opened, and under the action of the air suction pump, the cooling air flows in from the cooling air port 344 to the piston rod. 331 and adsorption sieve cylinder 332 for cooling.
根据一个实施例，吸附器330与活塞腔341之间设有多个O形的密封圈335。According to one embodiment, a plurality of O-shaped sealing rings 335 are disposed between the adsorber 330 and the piston cavity 341 .
根据一个实施例，解析缸体350的内壁设有衬管355。解析缸体350可采用不锈钢制作，解析缸体350密封嵌入化学性质稳定的聚四氟乙烯材料制成的衬管355，衬管355可定期更换，一方面能保证样品气不与金属材料接触、反应并由此导致的检测样品和检测信号的失真，另一方面还可阻挡大颗粒物质掉入色谱柱并堵塞色谱柱。According to one embodiment, the inner wall of the resolution cylinder 350 is provided with a liner 355 . The analysis cylinder 350 can be made of stainless steel. The analysis cylinder 350 is sealed and embedded with a liner 355 made of polytetrafluoroethylene material with stable chemical properties. The liner 355 can be replaced regularly. On the one hand, it can ensure that the sample gas does not come into contact with metal materials. The reaction and the resulting distortion of the detection sample and detection signal, on the other hand, can also prevent large particles from falling into the chromatographic column and clogging the chromatographic column.
优选的，在吸附筛筒332的底部设置一个绝热垫333，用于隔绝解析腔356的热，避免解析腔356中的热量传导到吸附筛筒332中。优选的，吸附筛筒332的底部为敞口，绝热垫333与吸附筛筒332通过螺纹连接。拔出吸附器330或拧下活塞缸体340，并旋开位于吸附器330底部的绝热垫可对吸附剂进行更换。用户可根据不同的检测目的选择吸附剂类型(填充吸附剂的直径应大于吸附筛筒332的网孔孔径)，极大地提高了仪器的灵活性。绝热垫可采用隔热性能好的聚四 氟材料，绝热垫能有效保证吸附器330采样富集时吸附筛筒332和吸附剂处于近乎室温，有利于样品吸附和富集。Preferably, a heat insulating pad 333 is provided at the bottom of the adsorption sieve cylinder 332 to insulate the heat of the desorption chamber 356 and prevent the heat in the desorption chamber 356 from being transferred to the adsorption sieve cylinder 332 . Preferably, the bottom of the adsorption sieve cylinder 332 is open, and the heat insulating pad 333 is connected to the adsorption sieve cylinder 332 through threads. Pull out the adsorber 330 or unscrew the piston cylinder 340, and unscrew the heat insulating pad at the bottom of the adsorber 330 to replace the adsorbent. The user can select the type of adsorbent according to different detection purposes (the diameter of the filled adsorbent should be larger than the mesh aperture of the adsorption screen cylinder 332), which greatly improves the flexibility of the instrument. The thermal insulation pad can be made of polytetrafluoroethylene material with good thermal insulation performance. The thermal insulation pad can effectively ensure that the adsorption screen cylinder 332 and the adsorbent are at nearly room temperature when the adsorber 330 is sampling and enriching, which is conducive to sample adsorption and enrichment.
优选的，本实用新型中的吸附器330的活塞杆331及吸附筛筒332一体制成，且采用化学性质稳定的耐热型材料制成，如聚四氟。活塞缸体340可采用强度大、耐热好、化学性质稳定的聚四氟材料制作。为了使吸附器330能够稳定地沿活塞腔341移动，活塞腔341中设置密封导轨，为取样、富集、风冷、热解析进样提供支撑及密封管路。Preferably, the piston rod 331 and the adsorption sieve cylinder 332 of the adsorber 330 in the present utility model are integrally made, and are made of heat-resistant materials with stable chemical properties, such as polytetrafluoroethylene. The piston cylinder 340 can be made of polytetrafluoro material with high strength, good heat resistance and stable chemical properties. In order to enable the adsorber 330 to move stably along the piston cavity 341 , a sealed rail is provided in the piston cavity 341 to provide support and sealed pipelines for sampling, enrichment, air cooling, and thermal desorption sampling.
参照图8所示，为了说明方便，两个吸附器中，图中左边的吸附器为第一吸附器，以图中右边的吸附器为第二吸附器。在需对被检物进行采样时，首先将解析缸体外壁的加热膜打开，设置好温度，待温度稳定后先将两个吸附器都摁入解析腔内进行吸附剂净化，然后将两个吸附器拉起，将其中第一吸附器拉至如图8所示的左侧吸附器所在位置，将第二吸附器拉高至吸附筛筒上部略低于活塞缸体上部样品进气口的位置(不形成抽气通路，同时有助于吸附器冷却及后期样品吸附)，开启采样吸气泵电源，将采样器的喇叭采样头近距离对准被检物，在吸气泵的作用下开始收集被检物挥发性气体，持续采用3-5分钟，以实现取样品富集，待样品富集后将位于第一吸附器的吸附筛筒全部摁入解析腔中进行样品析出，与此同时将第二吸附器再次拉高直至样品进气口、吸附筛筒和吸气泵气口形成连通气路的位置，如此循环操作以实现有多个被检物时的全时、快速样品收集和富集解析。被析出的被检样品与从载气入口进入的载气迅速均匀混合后进入样品排出口，实现了样品的解析进样，样品排出口与检测设备或者分离设备相连接。Referring to Fig. 8, for convenience of description, among the two adsorbers, the adsorber on the left in the figure is the first adsorber, and the adsorber on the right in the figure is the second adsorber. When it is necessary to sample the object to be tested, first open the heating film on the outer wall of the analysis cylinder, set the temperature, and after the temperature is stable, press both adsorbers into the analysis chamber for adsorbent purification, and then put the two Pull up the adsorber, pull the first adsorber to the position of the left adsorber as shown in Figure 8, and pull the second adsorber to the point where the upper part of the adsorption sieve cylinder is slightly lower than the sample inlet on the upper part of the piston cylinder. position (does not form a suction path, and at the same time contributes to the cooling of the adsorber and the subsequent sample adsorption), turn on the power of the sampling aspirator pump, and align the horn sampling head of the sampler with the sample at a close distance to the object under the action of the aspirator pump. Start to collect the volatile gas of the detected object, and continue to use it for 3-5 minutes to achieve sample enrichment. After the sample is enriched, press all the adsorption sieve cylinders located in the first adsorber into the analysis chamber for sample precipitation. At the same time, the second adsorber is pulled up again until the position where the sample inlet, the adsorption sieve cylinder and the air port of the suction pump form a communication air path, so that the cycle operation can realize full-time and rapid sample collection and monitoring when there are multiple analytes. Enrichment analysis. The precipitated sample to be tested is quickly and uniformly mixed with the carrier gas entering from the carrier gas inlet, and then enters the sample discharge port to realize the analysis and injection of the sample, and the sample discharge port is connected with the detection equipment or separation equipment.
图9是根据本实用新型检测设备的样品分析装置400的一个实施例的总体结构示意图。样品分析装置400可以大体包括样品导入装置部分和离子迁移谱分析装置部分。FIG. 9 is a schematic diagram of an overall structure of an embodiment of a sample analysis device 400 of the detection device of the present invention. The sample analysis device 400 may generally include a sample introduction device portion and an ion mobility spectrometry device portion.
样品导入装置包括集束毛细管柱401，集束毛细管柱401包括多个毛细管柱。在一种实施例中，集束毛细管柱401可以通过将多根独立的单根毛细管柱平行地集聚成一束构成。在一种实施例中，集束毛 细管柱401可以通过在一根柱子上形成多个平行的毛细孔构成。在一种实施例中，集束毛细管柱401由非金属材料形成。例如，通常情况，毛细管柱可以由玻璃材料形成。毛细管柱也可以由其他材料形成。集束毛细管柱401配置成具有大体平齐的入口端和出口端。一支集束毛细管由成百上千根平行毛细管柱构成，例如500-5000根平行毛细管柱集成在一个横截面为正六边形的玻璃柱内，每根毛细管柱的内径为20-100μm，一般为～40μm。在每根毛细管柱的内表面可以涂覆一层固定相，固定相的选择可以根据需要进行选择。由于集束毛细管柱401强大的分离能力，通常可做成尺寸较短的笔形柱(40-250mm)即可以实现分离的功能。尺寸较长的柱可绕成圆盘形。混合样品组分经过与毛细管固定相之间的相互作用以保留时间不同实现物质的分离。毛细管柱的保留时间在秒-分钟量级(一般为几十秒～几分钟，最小峰宽几秒)。The sample introduction device includes a bundled capillary column 401, and the bundled capillary column 401 includes a plurality of capillary columns. In one embodiment, the bundled capillary column 401 can be formed by arranging a plurality of independent single capillary columns in parallel into a bundle. In one embodiment, the bundled capillary column 401 can be formed by forming a plurality of parallel capillary holes on a column. In one embodiment, bundled capillary column 401 is formed of a non-metallic material. For example, typically, capillary columns may be formed from glass materials. Capillary columns can also be formed from other materials. Clustered capillary column 401 is configured with substantially flush inlet and outlet ends. A cluster capillary consists of hundreds or thousands of parallel capillary columns, for example, 500-5000 parallel capillary columns are integrated in a glass column with a regular hexagonal cross-section, and the inner diameter of each capillary column is 20-100 μm, generally ~40μm. A layer of stationary phase can be coated on the inner surface of each capillary column, and the choice of stationary phase can be selected according to needs. Due to the powerful separation capability of the bundled capillary column 401, it can usually be made into a shorter pencil-shaped column (40-250 mm) to achieve the separation function. Columns with longer dimensions can be wound into a disc shape. The mixed sample components are separated by different retention times through the interaction with the capillary stationary phase. The retention time of the capillary column is on the order of seconds to minutes (generally tens of seconds to several minutes, and the minimum peak width is several seconds).
集束毛细管柱401的结构具有如下优点：1)集聚上千根毛细管柱，使集束毛细管柱401的容量更大，可以用来得到更高的灵敏度；2)集束毛细管柱401的毛细管柱的更细，例如毛细管柱可以具有内径20-100μm，而传统的毛细柱内径在0.25-0.53mm之间，因而集束毛细管柱401的毛细管柱有更好的分离效果，可以用比较短的尺寸实现很好的分离；3)笔形的集束毛细管柱401(40-250mm)允许通过的压力梯度比常规毛细管柱(一般30m)小，因此集束毛细管柱401内的流速是传统毛细管柱流速的2-3个量级，而且具有更高的流量范围(20-150ml/min)，因此集束毛细管柱401不但允许快速分离，而且允许等温分离。基于这些优势一方面可实现集束毛细管柱401-离子迁移谱联用谱仪近似于实时分离检测的能力，另一方面集束毛细管短小的尺寸帮助实现便携式的集束毛细管柱-离子迁移谱仪。The structure of the clustered capillary column 401 has the following advantages: 1) thousands of capillary columns are gathered, so that the capacity of the clustered capillary column 401 is larger, which can be used to obtain higher sensitivity; 2) the capillary column of the clustered capillary column 401 is thinner For example, the capillary column can have an inner diameter of 20-100 μm, while the inner diameter of the traditional capillary column is between 0.25-0.53 mm, so the capillary column of the bundled capillary column 401 has a better separation effect, and can achieve a good separation effect with a relatively short size. Separation; 3) The pressure gradient allowed by the pencil-shaped clustered capillary column 401 (40-250mm) is smaller than that of the conventional capillary column (generally 30m), so the flow velocity in the clustered capillary column 401 is 2-3 orders of magnitude of the traditional capillary column flow rate , and has a higher flow range (20-150ml/min), so the bundled capillary column 401 not only allows rapid separation, but also allows isothermal separation. Based on these advantages, on the one hand, the ability of the cluster capillary column 401-ion mobility spectrometer to approximate real-time separation and detection can be realized. On the other hand, the short size of the cluster capillary helps to realize the portable cluster capillary column-ion mobility spectrometer.
为了加强玻璃柱的保护，提高集束毛细管柱整体强度，防止意外破碎，样品导入装置还包括配置成包围并保护集束毛细管柱401的金属圆套420。在本实用新型的图9中示出了正六边形玻璃柱外周耦合一个金属圆套420的情形，即笔形玻璃集束毛细管柱401的横截为正六边形。集束毛细管柱401的其他形状的截面也是可以的，例如圆形 的。In order to strengthen the protection of the glass column, improve the overall strength of the bundled capillary column, and prevent accidental breakage, the sample introduction device further includes a metal sleeve 420 configured to surround and protect the bundled capillary column 401 . In FIG. 9 of the present utility model, the situation that a regular hexagonal glass column is coupled with a metal sleeve 420 is shown, that is, the cross section of the pen-shaped glass bundled capillary column 401 is a regular hexagon. Other shaped cross-sections of the bundled capillary column 401 are also possible, for example circular.
样品导入装置还包括温控系统，温控系统与集束毛细管柱401结合用于控制集束毛细管柱401内的温度。The sample introduction device also includes a temperature control system, which is combined with the bundled capillary column 401 to control the temperature inside the bundled capillary column 401 .
具体地，样品导入装置的温控系统包括导热体402，导热体402配置成直接接触包围集束毛细管柱401的金属圆套420。温控系统还包括嵌入在导热体402内的至少一个加热器404和至少一个传感器405。至少一个加热器404和至少一个传感器405的配合可以实现对导热体402的温度控制。加热器可以选多种形式。例如，可以在导热体402中嵌入多根加热棒404，例如嵌入1根或多根加热棒404，例如2、3、4、5、6、7、8、9、10根或更多根加热棒404。多根加热棒404可以均匀地分布在导热体402中以便更迅速且均匀地升高导热体402的温度。图9示出一根导热棒的情形。导热体402可以嵌入热丝，热丝的布置也有利于均匀的加热，例如可以使得导热体402本身类似一种可升温的加热体。Specifically, the temperature control system of the sample introduction device includes a thermal conductor 402 configured to directly contact the metal sleeve 420 surrounding the bundled capillary column 401 . The temperature control system further includes at least one heater 404 and at least one sensor 405 embedded in the heat conductor 402 . The cooperation of at least one heater 404 and at least one sensor 405 can realize the temperature control of the heat conductor 402 . The heater can be selected in various forms. For example, multiple heating rods 404 can be embedded in the heat conductor 402, such as one or more heating rods 404, such as 2, 3, 4, 5, 6, 7, 8, 9, 10 or more heating rods 404 can be embedded. Stick 404. A plurality of heating rods 404 can be evenly distributed in the heat conducting body 402 so as to increase the temperature of the heat conducting body 402 more quickly and uniformly. Figure 9 shows the situation of a heat conducting rod. The heat conductor 402 can be embedded with a heating wire, and the arrangement of the heat wire is also conducive to uniform heating, for example, the heat conductor 402 itself can be made like a heating body that can be heated.
在一个实施例中，传感器405可以设置在靠近金属圆套420附近，以便使传感器405所测的温度更接近毛细管柱内的温度。多个传感器405可以均匀地分布在导热体402的靠近金属圆套420周围。In one embodiment, the sensor 405 can be arranged near the metal sleeve 420 so that the temperature measured by the sensor 405 is closer to the temperature inside the capillary column. A plurality of sensors 405 may be evenly distributed around the heat conductor 402 near the metal sleeve 420 .
在一个实施例中，导热体402包括导热体402外周上的多个凸起430，在导热体402外周的多个凸起430之间形成空间403。这些空间可以看作沟槽403，也可以看作流体通过的通道403，如图10所示。In one embodiment, the heat conductor 402 includes a plurality of protrusions 430 on the outer periphery of the heat conductor 402 , and a space 403 is formed between the plurality of protrusions 430 on the outer periphery of the heat conductor 402 . These spaces can be regarded as grooves 403, and can also be regarded as channels 403 through which fluid passes, as shown in FIG. 10 .
每个凸起430的尺寸可以相同，也可以不同。单个凸起430之间的间距可以相同，也可以不同。例如一部分凸起430尺寸大，其他的凸起430尺寸小。例如两列凸起430一组，每组凸起430之间的间距比每组的两个突起之间的间距大。凸起430的布置也可以是不均匀的。本领域即使人员应该知道，包括凸起430的其他尺寸和间距的凸起430的布置也是可以的。The size of each protrusion 430 can be the same or different. The spacing between individual protrusions 430 can be the same or different. For example, some protrusions 430 are large in size, while other protrusions 430 are small in size. For example, there are two rows of protrusions 430 in one group, and the distance between each group of protrusions 430 is larger than the distance between two protrusions in each group. The arrangement of the protrusions 430 may also be non-uniform. Arrangements of the protrusions 430 including other sizes and spacings of the protrusions 430 are also possible, even those skilled in the art will appreciate.
换句话说，导热体402可以看作两部分，一部分是导热体402的基部，另一部分是导热体402的凸起430。在一个实施例中，基部的径向厚度可以较小，凸起430的高度可以较大。导热体402上的多个凸起430有利于流体在凸起430之间流动以与导热体402交换热。在 一个实施例中，例如，通入气体使得气体在多个凸起430之间流动，可以加速导热体402的多个凸起430与通入的气体热交换，此时多个凸起430可以用作散热片。在一个实施例中，多个凸起430之间可以缠绕管道，管道内可以流过流体，通过高温流体或低温流体可以实现流体的管道与导热体402进行热交换，从而控制导热体402的温度。In other words, the heat conductor 402 can be regarded as two parts, one part is the base of the heat conductor 402 , and the other part is the protrusion 430 of the heat conductor 402 . In one embodiment, the radial thickness of the base can be smaller and the height of the protrusion 430 can be larger. The plurality of protrusions 430 on the heat conducting body 402 facilitate fluid flow between the protrusions 430 to exchange heat with the heat conducting body 402 . In one embodiment, for example, passing gas to make the gas flow between the plurality of protrusions 430 can accelerate the heat exchange between the plurality of protrusions 430 of the heat conductor 402 and the passing gas, and at this time, the plurality of protrusions 430 can Used as a heat sink. In one embodiment, pipes can be wound between the protrusions 430, fluid can flow through the pipes, and heat exchange between the pipes of the fluid and the heat conductor 402 can be realized through high-temperature fluid or low-temperature fluid, thereby controlling the temperature of the heat conductor 402 .
在一个实施例中，导热体402的基部厚度较薄，在多个凸起430之间布置加热膜，由此可以实现导热体402的升温；同时，在多个凸起430之间布置热媒流体的管道实现经由热传递的降温。由此配置，结合传感器405可以迅速地控制导热体402的温度。In one embodiment, the thickness of the base of the heat conductor 402 is relatively thin, and a heating film is arranged between the plurality of protrusions 430 , so that the temperature of the heat conductor 402 can be increased; at the same time, a heat medium is arranged between the plurality of protrusions 430 The piping of the fluid achieves cooling via heat transfer. With this configuration, the temperature of the thermal conductor 402 can be quickly controlled in conjunction with the sensor 405 .
由于多个凸起430的设置，可以看作导热体402具有用于容纳流动的热媒流体或热媒流体管道以便温度传递的沟槽。具体地，图12示出流体管道缠绕在多个凸起430之间的情形。热媒流体管道可以蜿蜒穿过多个凸起430，或者热媒流体管道可以螺旋地围绕导热体402的多个凸起430之间，由此热媒流体管道与导热体402之间进行热传递。应该理解，可以以任何方式将流体管道布置在由多个凸起430构成的通道或沟道之中，凸起430此时不但与热媒管道进行热交换，还起到支撑管道的作用。Due to the arrangement of the plurality of protrusions 430, it can be seen that the heat conductor 402 has grooves for accommodating flowing heat medium fluid or heat medium fluid pipes for temperature transfer. Specifically, FIG. 12 shows a situation where a fluid conduit is wound between a plurality of protrusions 430 . The heat medium fluid pipeline can meander through a plurality of protrusions 430, or the heat medium fluid pipeline can spirally surround between the plurality of protrusions 430 of the heat conductor 402, so that heat is carried out between the heat medium fluid pipeline and the heat conductor 402. transfer. It should be understood that the fluid pipes may be arranged in any manner in the channels or channels formed by the plurality of protrusions 430 , and the protrusions 430 not only perform heat exchange with the heat medium pipes, but also play a role of supporting the pipes.
在一个实施例中，多个凸起430是有利的，多个凸起430可以看作散热凸起430，用流体直接散热；多个凸起430可以用于限定流体通道的布置，将流体通道绕在多个凸起之间，可以固定流体通道的位置。In one embodiment, a plurality of protrusions 430 are advantageous, and the plurality of protrusions 430 can be regarded as heat dissipation protrusions 430, and the heat dissipation can be directly performed by the fluid; Wrapped between a plurality of protrusions, the position of the fluid channel can be fixed.
在本实用新型的另一实施例中，样品导入装置还可以包括外壳406，外壳406包围温控系统。在一个实施例中，样品导入装置还可以包括保温层408，保温层408设置在外壳406和导热体402之间。在一个实施例中，外壳406可以以密封的方式包围导热体402的外侧面。当保温层408和外壳406包围导热体402时，导热体402上的多个凸起可以用以支撑保温层408和外壳406。如图9所示，在多个凸起和保温层408之间形成了许多通道。热媒流体的管道可以穿过这些通道或上面所说的沟槽而布置在导热体402的外周上，以便进行充分的热传递。In another embodiment of the present utility model, the sample introduction device may further include a housing 406, and the housing 406 surrounds the temperature control system. In one embodiment, the sample introducing device may further include an insulating layer 408 disposed between the housing 406 and the heat conductor 402 . In one embodiment, the housing 406 may enclose the outer side of the thermal conductor 402 in a sealed manner. When the insulation layer 408 and the shell 406 surround the heat conductor 402 , the plurality of protrusions on the heat conductor 402 can be used to support the heat insulation layer 408 and the shell 406 . As shown in FIG. 9 , a plurality of channels are formed between the plurality of protrusions and the insulating layer 408 . Pipes for the heat medium fluid may be arranged on the outer periphery of the heat conducting body 402 through these channels or the above-mentioned grooves for sufficient heat transfer.
在一个实施例中，可以设置气泵418，通过管道417通入到上述沟槽403内，气泵418通入加压气体进入多个凸起430之间的沟槽403，帮助导热体402的冷却或升温。在一个实施例中，可以直接将液体通入由多个凸起430形成的沟槽中实现热交换。In one embodiment, an air pump 418 can be provided, which is passed into the above-mentioned groove 403 through the pipeline 417, and the air pump 418 passes pressurized gas into the groove 403 between the plurality of protrusions 430 to help the cooling of the heat conductor 402 or heat up. In one embodiment, the heat exchange can be realized by directly passing the liquid into the grooves formed by the plurality of protrusions 430 .
在一个实施例中，集束毛细管柱401的入口端伸出到样品导入装置的外壳406之外。金属圆套420的一部分也可以随着集束毛细管柱401一起伸出到外壳406之外。In one embodiment, the inlet end of the bundled capillary column 401 protrudes beyond the housing 406 of the sample introduction device. A part of the metal sleeve 420 can also protrude out of the housing 406 together with the bundled capillary column 401 .
由于集束毛细管柱401中的样品流速比常规气相色谱柱的快，因此样品导入装置与离子迁移谱分析装置的接口尤为重要。样品导入装置与离子迁移谱分析装置的接口的作用是将集束毛细管柱401快速分离的样品无损地、平稳地引入离子迁移谱分析装置的反应区内。Since the sample flow rate in the clustered capillary column 401 is faster than that of a conventional gas chromatography column, the interface between the sample introduction device and the ion mobility spectrometry analysis device is particularly important. The function of the interface between the sample introducing device and the ion mobility spectrometry device is to introduce the sample rapidly separated by the clustered capillary column 401 into the reaction area of the ion mobility spectrometry device without damage and smoothly.
在一个实施例中，样品分析装置400还包括隔热定位装置411，配置成能够在样品导入装置和离子迁移谱分析装置之间连接样品导入装置和离子迁移谱分析装置，并且隔断样品导入装置和离子迁移谱分析装置之间的热传递，以便样品导入装置和离子迁移谱分析装置的分别的独立温度控制。In one embodiment, the sample analysis device 400 further includes a thermal insulation positioning device 411 configured to connect the sample introduction device and the ion mobility spectrometry analysis device between the sample introduction device and the ion mobility spectrometry analysis device, and isolate the sample introduction device from the ion mobility spectrometry analysis device. Heat transfer between the ion mobility spectrometry device for separate independent temperature control of the sample introduction device and the ion mobility spectrometry device.
在一个实施例中，隔热定位装置411包括与样品导入装置的出口端连接的第一连接端和与离子迁移谱分析装置的样品导入口连接的第二连接端。具体地，第一连接端连接并密封在集束毛细管柱401的一个端部，第二连接端的形状与离子迁移分析装置的腔的开口的形状互补。隔热定位装置411的形状如图9和图11的截面图所示。隔热定位装置411具有阶梯状的形状，图11分别示出沿B-B和C-C线的截面图。在一个实施例中，在隔热定位装置411的部分的外表面上可以设置垫圈。垫圈413可以起到密封作用，当样品导入装置插入离子迁移谱分析装置时，隔热定位装置411连接在两者之间，良好的密封是必要的，以避免反应区414中的粒子泄漏或外界气体进入反应区414影响测量的精度。In one embodiment, the thermal insulation positioning device 411 includes a first connection end connected to the outlet port of the sample introduction device and a second connection end connected to the sample introduction port of the ion mobility spectrometry analysis device. Specifically, the first connection end is connected and sealed to one end of the cluster capillary column 401 , and the shape of the second connection end is complementary to the shape of the opening of the chamber of the ion mobility analysis device. The shape of the heat insulation positioning device 411 is shown in the sectional views of Fig. 9 and Fig. 11 . The heat insulation positioning device 411 has a stepped shape, and FIG. 11 shows cross-sectional views along lines B-B and C-C, respectively. In one embodiment, a gasket may be provided on the outer surface of the portion of the insulating positioning means 411 . The gasket 413 can play a sealing role. When the sample introduction device is inserted into the ion mobility spectrometry device, the heat-insulating positioning device 411 is connected between the two. Good sealing is necessary to avoid particle leakage in the reaction zone 414 or external Gas entering the reaction zone 414 affects the accuracy of the measurement.
隔热定位装置411可以由塑料材料形成，例如由PEEK，聚四氟乙烯形成。隔热定位装置411由可以其他耐高温和绝热的非金属材料形成。例如耐火材料和石棉等材料形成。通过隔热定位装置411，非 金属材料形成的集束毛细管柱401的出口端通过离子迁移谱分析装置的样品导入口直接插入离子迁移谱分析装置的腔内，即离子迁移谱分析装置的反应区414内，同时避免金属圆套420靠近离子迁移谱分析装置的离子区，从而避免金属圆套420干扰离子迁移谱分析装置的精度。具体地，金属圆套420不进入离子迁移谱分析装置的样品导入口。优选地，金属圆套420远离离子迁移谱分析装置的样品导入口。The thermal insulation positioning device 411 may be formed of plastic material, such as PEEK, polytetrafluoroethylene. The heat insulation positioning device 411 is formed of other high temperature resistant and heat insulating non-metallic materials. Materials such as refractories and asbestos are formed. Through the heat insulation positioning device 411, the outlet end of the clustered capillary column 401 formed by non-metallic materials is directly inserted into the chamber of the ion mobility spectrometry analysis device through the sample introduction port of the ion mobility spectrometry analysis device, that is, the reaction zone 414 of the ion mobility spectrometry analysis device At the same time, the metal sleeve 420 is prevented from being close to the ion region of the ion mobility spectrometer analysis device, thereby preventing the metal sleeve 420 from interfering with the accuracy of the ion mobility spectrometry analysis device. Specifically, the metal sleeve 420 does not enter the sample introduction port of the ion mobility spectrometry device. Preferably, the metal sleeve 420 is far away from the sample introduction port of the ion mobility spectrometry device.
通过这样的配置，样品样品可以直接送入离子迁移谱分析装置的反应区414内，避免现有技术中气体物质被引入到电离区415内被(例如)高能射线打成离子碎片的问题。同时，气体物质能够被毛细管柱分离，满足分析的要求，直接被送入反应区414分析。Through this configuration, the sample can be directly sent into the reaction zone 414 of the ion mobility spectrometry device, avoiding the problem in the prior art that gaseous substances are introduced into the ionization zone 415 and are broken into ion fragments by (for example) high-energy rays. At the same time, the gaseous substances can be separated by the capillary column to meet the analysis requirements, and are directly sent to the reaction zone 414 for analysis.
在一个实施例中，隔热定位装置411可以与样品导入装置形成为一个整体，这在实际使用时也是有利的。在此情况下，隔热定位装置411可以密封样品导入装置的一端，样品导入装置的出口端从隔热定位装置411伸出，如图9所示。此时，包括隔热定位装置411的样品导入装置的出口端如图9所示，即由隔热定位装置411的端部包裹集束毛细管柱401，其中毛细管柱的部分由隔热定位装置411的非金属材料直接包裹。In one embodiment, the thermal insulation positioning device 411 can be integrated with the sample introduction device, which is also advantageous in practical use. In this case, the thermal insulation positioning device 411 can seal one end of the sample introduction device, and the outlet end of the sample introduction device protrudes from the thermal insulation positioning device 411 , as shown in FIG. 9 . At this time, the outlet end of the sample introduction device including the thermal insulation positioning device 411 is shown in FIG. Non-metallic materials are directly wrapped.
由于隔热定位装置411的设置，可以实现样品导入装置方便地直接插入到离子迁移谱分析装置的腔，即反应区414内。这在要求快速分析气体样品的场合下尤为重要。样品导入装置可以单独进行温度控制，在预备时间里可以单独控制样品导入装置的温度，在样品导入装置具备想要的温度条件下，将样品导入装置插入离子迁移谱分析装置；通过隔热定位装置411连接并确定样品导入装置和离子迁移谱分析装置之间的相对位置。由于隔热定位装置411的热绝缘性质和刚性，样品导入装置的温度不会影响离子迁移谱分析装置的测量精确，并且样品导入装置和离子迁移谱分析装置之间的位置关系可以确定。通过这样的配置，可以方便地进行样品导入装置和离子迁移谱分析装置的连接和分离，这在实际检查过程具有积极的意义，极大地方便检查不同的样品，并且并于运输，整体检查系统的体积减小。例如，可以配备多个样品导入装置，方便检查不同的样品，加快检查的速度和 精确度。Due to the setting of the heat-insulating positioning device 411 , the sample introduction device can be directly inserted into the chamber of the ion mobility spectrometry device, that is, the reaction zone 414 . This is especially important where rapid analysis of gas samples is required. The temperature of the sample introduction device can be controlled independently, and the temperature of the sample introduction device can be controlled separately during the preparation time. When the sample introduction device has the desired temperature condition, insert the sample introduction device into the ion mobility spectrometer analysis device; through the heat insulation positioning device 411 connects and determines the relative position between the sample introduction device and the ion mobility spectrometry analysis device. Due to the thermal insulation properties and rigidity of the insulating positioning device 411, the temperature of the sample introducing device will not affect the measurement accuracy of the ion mobility spectrometry device, and the positional relationship between the sample introducing device and the ion mobility spectrometry device can be determined. Through such a configuration, the connection and separation of the sample introduction device and the ion mobility spectrometry analysis device can be conveniently carried out, which is of positive significance in the actual inspection process, which greatly facilitates the inspection of different samples, and is convenient for transportation, and the overall inspection system Reduced in size. For example, multiple sample introduction devices can be equipped to facilitate the inspection of different samples and speed up the inspection speed and accuracy.
在一个实施例中，集束毛细管柱401的金属圆套420的长度配置成当集束毛细管柱401插入到离子迁移谱分析装置的腔414内时金属圆套420不进入离子迁移谱分析装置的电离区415。金属圆套420的端部终止在隔热定位装置411中，例如如图9所示的位置。然而，应该知道金属圆套420的位置可以是其他情形，只要金属圆套420不接近包含离子的反应区414即可。例如，金属圆套420不进入，或远离离子迁移谱分析装置的样品导入口。In one embodiment, the length of the metal sleeve 420 of the clustered capillary column 401 is configured such that the metal sleeve 420 does not enter the ionization region of the ion mobility spectrometry device when the clustered capillary column 401 is inserted into the chamber 414 of the ion mobility spectrometry device 415. The end of the metal sleeve 420 terminates in the insulating positioning device 411 , for example as shown in FIG. 9 . However, it should be understood that the position of the metal sleeve 420 can be other situations, as long as the metal sleeve 420 is not close to the reaction zone 414 containing ions. For example, the metal sleeve 420 does not enter or is away from the sample introduction port of the ion mobility spectrometry device.
在一个实施例中，样品分析装置400包括用于分析样品导入装置导入的样品的离子迁移谱分析装置。离子迁移谱分析装置包括用于气体反应的腔414。腔414包括样品导入口，用以导入待分析的样品。离子迁移谱分析装置还包括电离区415。In one embodiment, the sample analysis device 400 includes an ion mobility spectrometry analysis device for analyzing a sample introduced by the sample introduction device. The ion mobility spectrometry device includes a chamber 414 for gas reactions. The cavity 414 includes a sample introduction port for introducing a sample to be analyzed. The ion mobility spectrometry device also includes an ionization region 415 .
如图9所示，样品导入装置位于离子迁移谱分析装置的上侧，电离区415的位置在下侧。根据本实用新型的一个实施例，样品导入装置与离子迁移谱分析装置的电离区415相对地布置是有利的。与现有技术中样品样品通入电离区415电离的技术思路不同，本实用新型的样品导入装置配置成使得要分析的样品避开电离区415，将要分析的样品样品直接导入至反应区414中，这有利地避免了分子离子碎片的产生，避免了现有技术将样品导入到电离区415中带来的例如样品被打成碎片等其他问题，例如由于非直线型的气体通道带来的湍流等。即，实现快速分离样品样品的同时将样品样品平稳地引入至离子迁移谱分析装置。As shown in FIG. 9 , the sample introduction device is located on the upper side of the ion mobility spectrometry device, and the ionization region 415 is located on the lower side. According to an embodiment of the present invention, it is advantageous that the sample introduction device is arranged opposite to the ionization region 415 of the ion mobility spectrometry device. Different from the technical thinking in the prior art that the sample is passed into the ionization zone 415 for ionization, the sample introduction device of the present invention is configured so that the sample to be analyzed avoids the ionization zone 415, and the sample to be analyzed is directly introduced into the reaction zone 414 , which advantageously avoids the generation of molecular ion fragments, and avoids other problems such as the sample being broken into fragments caused by introducing the sample into the ionization region 415 in the prior art, such as the turbulent flow caused by the non-linear gas channel wait. That is, the rapid separation of the sample sample is achieved while the sample sample is smoothly introduced into the ion mobility spectrometry device.
在本实用新型的一个实施例中，离子迁移谱分析装置412为正422、负423双模式迁移管，反应区414在正模式管422和负模式管423之间，电离区415和反应区414分开布置，且通过可闭合的开口连接，如图9示出一种布置。例如，电离区415在反应区414一侧的附近。In one embodiment of the present utility model, the ion mobility spectrometry analysis device 412 is positive 422, negative 423 dual-mode transfer tubes, the reaction zone 414 is between the positive mode tube 422 and the negative mode tube 423, the ionization zone 415 and the reaction zone 414 Arranged separately and connected by a closable opening, one arrangement is shown in FIG. 9 . For example, the ionization region 415 is near the side of the reaction region 414 .
根据本实用新型的设计思路，在一个实施例中，例如空气的载气416被导入电离区415内，载气在电离区415被离化，生成带电载气，例如H+(H2O)n，和O2-(H2O)n。带电的载气被送入反应区中，在 此带电的载气与样品结合发生反应，从而使样品分子带正电或负电。这与现有技术将样品气体与载气混合一起被离化不同。例如，生物大分子与水合质子或水合氧离子结合形成带正电或负电的分子，而不是被电离成分子碎片。正模式迁移管422及负模式迁移管423均包括离子门424、迁移区、抑制栅427和法拉第盘428。迁移区可以由一串不锈钢保护环425和陶瓷绝缘环426串接而成。带正电的样品粒子在正模式迁移管中检测，带负电的样品粒子在负模式迁移管中检测。According to the design concept of the present invention, in one embodiment, the carrier gas 416 such as air is introduced into the ionization region 415, and the carrier gas is ionized in the ionization region 415 to generate a charged carrier gas, such as H+ (H2 O)n , and O2− (H2 O)n . The charged carrier gas is fed into the reaction zone where it reacts with the sample binding to positively or negatively charge the sample molecules. This is different from the prior art where the sample gas is mixed with the carrier gas and ionized. For example, biological macromolecules combine with hydrated protons or hydrated oxygen ions to form positively or negatively charged molecules, rather than being ionized into molecular fragments. Both the positive mode transfer tube 422 and the negative mode transfer tube 423 include an ion gate 424 , a transfer region, a suppression grid 427 and a Faraday disk 428 . The migration area can be formed by a series of stainless steel protection rings 425 and ceramic insulating rings 426 connected in series. Positively charged sample particles are detected in the positive mode transfer tube and negatively charged sample particles are detected in the negative mode transfer tube.
具体地，离子迁移谱分析装置的载气416在电离区415被电离而生成反应离子，反应离子在离子迁移谱分析装置的载气416的吹扫下电离区415的载气入口进入反应区414，在反应区414与经集束毛细管柱401分离的样品相遇，发生亲电吸附反应，使样品分子吸附反应离子而带电性，正、负带电离子在迁移管正、负电场的推动作用下分别进入正、负迁移管422、423被分离，并被两端的法拉第盘428检测。离子迁移谱分析装置412的其他某些设计和原理可以参考申请第200810119974.6号，该专利申请的内容在此通过参考并入。Specifically, the carrier gas 416 of the ion mobility spectrometry device is ionized in the ionization region 415 to generate reaction ions, and the reaction ions enter the reaction region 414 at the carrier gas inlet of the ionization region 415 under the purging of the carrier gas 416 of the ion mobility spectrometry device , in the reaction zone 414 and the sample separated by the clustered capillary column 401 meet, an electrophilic adsorption reaction occurs, so that the sample molecules adsorb the reaction ions and become charged, and the positive and negative charged ions enter respectively under the promotion of the positive and negative electric fields of the transfer tube. Positive and negative transfer tubes 422, 423 are separated and detected by Faraday disks 428 at both ends. For some other designs and principles of the ion mobility spectrometry analysis device 412, reference may be made to application No. 200810119974.6, the content of which is hereby incorporated by reference.
下面简单描述根据本实用新型的检测设备的操作过程。The following briefly describes the operation process of the detection device according to the present invention.
可以将检测设备布置在例如机场、口岸、地铁站等场所，将采样装置的采样入口对准待检查的对象。采样装置中模拟的龙卷风式气流产生负压，将气相物质或颗粒物质吸入导风腔109中；经过半透膜111，样品与载气在混合区或混合腔中混合，通过进样口120排出。在样品进入预处理进样装置之前，将预处理进样装置的热解析腔的温度维持在一个合适的恒定高温(例如，80℃～300℃)，将吸附有样品的活塞式吸附器快速推至具有高温的热解析腔内，被推入热解吸腔中的吸附剂被迅速加热，吸附腔内吸附的样品在高温下瞬间析出，析出的样品与从热解析腔的载气入口引入的经预热的载气混合，最终被载气带入样品分析装置。样品分析装置中的毛细管柱束将样品分离，随后直接送入离子迁移谱分析装置。The detection equipment can be arranged in places such as airports, ports, subway stations, etc., and the sampling inlet of the sampling device is aimed at the object to be inspected. The tornado-like airflow simulated in the sampling device generates negative pressure, which sucks the gaseous phase or particulate matter into the air guide chamber 109; passes through the semi-permeable membrane 111, mixes the sample and carrier gas in the mixing area or mixing chamber, and discharges through the inlet 120 . Before the sample enters the pretreatment sampling device, the temperature of the thermal analysis chamber of the pretreatment sampling device is maintained at a suitable constant high temperature (for example, 80 ° C ~ 300 ° C), and the piston adsorber with the sample is quickly pushed Into the thermal analysis chamber with high temperature, the adsorbent pushed into the thermal desorption chamber is heated rapidly, and the sample adsorbed in the adsorption chamber is precipitated at high temperature instantly, and the precipitated sample is combined with the carrier gas introduced from the thermal analysis chamber. The preheated carrier gas is mixed and finally carried into the sample analysis device by the carrier gas. A capillary column bundle in the sample analysis unit separates the sample, which then feeds directly into the ion mobility spectrometry unit.
虽然本总体专利构思的一些实施例已被显示和说明，本领域普通技术人员将理解，在不背离本总体专利构思的原则和精神的情况下，可对这些实施例做出改变，本实用新型的范围以权利要求和它们的等 同物限定。Although some embodiments of the general patent concept have been shown and described, those skilled in the art will understand that changes can be made to these embodiments without departing from the principles and spirit of the general patent concept. The scope is defined by the claims and their equivalents.
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| CN201420871693.7UCN204424206U (en) | 2014-12-31 | 2014-12-31 | Checkout equipment |
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| CN201420871693.7UCN204424206U (en) | 2014-12-31 | 2014-12-31 | Checkout equipment |
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| CN204424206Utrue CN204424206U (en) | 2015-06-24 |
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| CN201420871693.7UExpired - LifetimeCN204424206U (en) | 2014-12-31 | 2014-12-31 | Checkout equipment |
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