A mass spectrometer gas sample pre-treatment device and system

Abstract

The present application relates to the field of gas pretreatment of mass spectrometer, and particularly relates to a pretreatment device and system for gas sample of mass spectrometer. The pretreatment device comprises a pipe body, a gas channel is arranged in the pipe body, a temperature control section is arranged in the middle of the pipe body, and connecting sections are arranged at both ends of the temperature control section; an electrically connected section is arranged outside the pipe body between the connecting section and the temperature control section, the electrically connected section is used for connecting an external power supply to electrically connect the pipe body, so that the pipe body generates heat; a refrigeration structure is arranged on the surface of the temperature control section. The efficiency of heat exchange in the refrigeration and heating process of the pretreatment device is greatly improved, so that the heat transfer and refrigeration efficiency is improved, and the power consumption is reduced. Moreover, the overall structure is simplified, the maintenance difficulty is reduced, the breakage of glass tubes and ceramic tubes used for insulation and isolation in the prior art under the condition of multiple cycles and high temperature changes is avoided, the maintenance frequency and maintenance cost are reduced, and the service life is prolonged.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of gas pretreatment of mass spectrometer, more particularly, to a pretreatment device and system of gas sample of mass spectrometer. BACKGROUND

[0002] The pretreatment of the gas sample for the mass spectrometer instrument used for precise detection has high requirements, and the purity of the gas sample is particularly important. The existing pretreatment principle of the gas sample is to use different stages of high temperature and ultra-low temperature to repeatedly capture adsorption and purge the gas sample according to the difference between the solubility point and the boiling point of the gas, so as to remove the non-detection object and leave enough target detection gas. However, in this process, the pretreatment device of the gas sample has high requirements for heating and refrigeration, the range of cold and hot change is large, and the speed of temperature regulation is required to be fast enough to realize the effective separation of the target detection gas in the gas sample. However, in the prior art, the structure of the pretreatment device is complex, and the temperature rising and falling speed is slow, which leads to low efficiency of the pretreatment process.

[0003] The existing pretreatment device structure generally includes a refrigeration part, a temperature guide pipe, a glass tube, a heating wire, a ceramic layer and a containing tube which are nested together from the outside to the inside. The refrigeration part is wound on the surface of the temperature guide pipe to form a refrigeration structure, and the heating wire is wound on the ceramic tube to form a heating structure, and the glass tube separates the refrigeration structure and the heating structure. In order to facilitate assembly, a certain gap is left between adjacent pipe bodies. However, this design causes the heat of the heating wire to not only need to pass through the ceramic tube, but also need to pass through the air layer to be transmitted to the containing tube in the heating process, and the cooling needs to pass through multiple air layers, glass tubes and heating structures to be transmitted to the containing tube. This leads to a very long temperature rising and falling cycle, and the single pretreatment cycle is close to 1 hour. In order to meet the detection requirements, the pretreatment is usually repeated without interruption for 24 hours a day, which has large power consumption. Moreover, due to the slow temperature rising and falling speed, the separation efficiency of the detection object is low, and the effect is not good. SUMMARY

[0004] The present application aims to overcome at least one of the above-mentioned defects of the prior art, and provides a pretreatment device and system of gas sample of mass spectrometer, which solves the problem of slow temperature regulation speed of the existing pretreatment device of mass spectrometer, leading to low pretreatment efficiency.

[0005] The technical scheme adopted by the present application is a pretreatment device of gas sample of mass spectrometer, comprising a pipe body, a gas channel is arranged in the pipe body, a temperature control section is arranged in the middle of the pipe body, and connecting sections are arranged at both ends of the temperature control section; an electrically conductive section is arranged outside the pipe body between the connecting section and the temperature control section, the electrically conductive section is used for connecting an external power source to electrify the pipe body to heat the pipe body; and a refrigeration structure is arranged on the surface of the temperature control section.

[0006] The pipe body is made of stainless steel, and one side of the pipe body for contacting the gas sample is provided with a passivation layer.

[0007] The surface of at least the temperature control section is provided with a ceramic layer.

[0008] The connecting section is provided with a first connecting piece made of polyimide, and the pipe body is connected to an external sampling channel through the first connecting piece.

[0009] The clamping section is provided with a second connecting piece between the power supply section and the temperature control section; the refrigeration structure layer includes a copper pipe sleeved outside the temperature control section and a refrigeration capillary pipe arranged on the copper pipe; one end of the second connecting piece is connected to the copper pipe, and the other end is connected to the clamping section, so that the pipe body and the copper pipe are separated by an annular separation space.

[0010] The second connecting piece is made of PEEK, the clamping section is provided with a high-temperature resistant heat-resistant layer, and the second connecting piece is connected to the clamping section through the high-temperature resistant heat-resistant layer.

[0011] The annular separation space extends into the second connecting piece and is connected to one end of the high-temperature resistant heat-resistant layer close to the temperature control section; the other end of the high-temperature resistant heat-resistant layer extends out of the other end of the second connecting piece away from the temperature control section.

[0012] The ceramic layer extends to the clamping section and protrudes from the side of the high-temperature resistant heat-resistant layer away from the temperature control section, the thickness of the ceramic layer is less than that of the high-temperature resistant heat-resistant layer, and the thickness of the annular separation space is 0.5% to 1% of the length of the pipe body.

[0013] Further provided is a mass spectrometer gas sample pretreatment system, comprising: a gas filtering device and a temperature control system, and the mass spectrometer gas sample pretreatment device; the temperature control system comprises: a controller and an electrically charged clamp power supply connected to the controller, a refrigeration device and a temperature measuring device; the electric clamp is connected to the power supply section, the refrigeration device is connected to the refrigeration structure, and the gas filtering device is connected to the connecting section, and the external gas sample enters the pipe body through the gas filtering device.

[0014] The surface of the temperature control section is provided with a ceramic layer, and the detection end of the temperature measuring device is connected to the surface of the ceramic layer.

[0015] Compared with the prior art, the application has the beneficial effects that the heat exchange efficiency in the refrigeration and heating process of the pretreatment device is greatly improved, the heat transfer and refrigeration efficiency are improved, and the power consumption is reduced. Moreover, the overall structure is simplified, the maintenance difficulty is reduced, the breakage of the glass tube and the ceramic tube for insulation and isolation in the prior art under the conditions of multiple cycles and high temperature changes is avoided, the maintenance frequency and cost are reduced, and the service life is prolonged. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 Figure 1 is a schematic view of the pretreatment device in the application.

[0017] Figure 2 Figure 2 is a sectional view of the pretreatment device in the application.

[0018] Figure 3 Figure 3 is an enlarged view of a part of the pretreatment device in the application.

[0019] Figure 4 Figure 4 is a schematic view of the electric clamp connected to the pretreatment device in the application.

[0020] The reference signs in the drawings: tube body 100, temperature control section 101, connecting section 102, power supply section 103, clamping section 104, gas passage 110, ceramic layer 120, refrigeration structure 200, copper tube 210, first connecting piece 300, second connecting piece 400, high-temperature-resistant heat-resistant layer 410, annular separation space 500, electric clamp 600. DETAILED DESCRIPTION

[0021] The drawings of the application are only used for illustrative description and cannot be understood as the limitation of the application. In order to better illustrate the following embodiments, some components in the drawings may be omitted, enlarged or reduced, and do not represent the actual product size; for those skilled in the art, it is understandable that some well-known structures and their descriptions in the drawings may be omitted.

[0022] Example 1

[0023] As Figure 1 and Figure 2As shown, the embodiment is a pretreatment device for a mass spectrometer gas sample, comprising a tube body 100, a gas channel 110 is arranged in the tube body 100, a temperature control section 101 is arranged in the middle of the tube body 100, and connecting sections 102 are arranged at both ends of the temperature control section 101; an energized section 103 is arranged outside the tube body 100 between the connecting section 102 and the temperature control section 101, the energized section 103 is used to connect an external power supply to the tube body 100 to make the tube body 100 heat up; and a refrigeration structure 200 is arranged on the surface of the temperature control section 101. The tube body 100 is used to accommodate the gas sample; the temperature control section 101 is used to heat the gas sample in the tube body 100 at a high temperature and extract the detected object by ultra-low temperature condensation; the connecting section 102 is used to connect the tube body 100 with a pipeline for external gas sample delivery; the energized section 103 is used to connect an external power supply to the tube body 100 to make the tube body 100 heat up; and the refrigeration structure 200 is used to refrigerate the temperature control section 101.

[0024] The tube body 100 is made of an electrically conductive and heat-generating material, or at least the temperature control section 101 is made of an electrically conductive and heat-generating material. The direct heating design of the tube body 100 overturns the existing multi-layer complex structure, and compared with the existing multi-layer design, it has a breakthrough in achieving high-speed heating, thereby improving the efficiency of impurity separation, greatly saving time, and enabling low-content components that were previously difficult to extract to be separated and detected. This design fully considers the subsequent detection conditions of the mass spectrometer gas sample, and since it does not rely on the heat transfer between the heating source and the tube body 100 or the heat conductivity between them, the heating speed is greatly improved, and the heating is uniform while the heating speed is improved.

[0025] The tube body 100 is made of stainless steel, and one side of the tube body 100 that is used to contact the gas sample is provided with a passivation layer. The passivation layer is used to form a contact protection layer with stable structure on the inner surface of the tube body 100.

[0026] The tube body 100 made of stainless steel utilizes the physical properties of the material on the one hand. As a slender and straight structure, the tube body 100 has high strength requirements, and the use of stainless steel material can avoid deformation and pressure resistance problems, and the hardness and cutting performance of stainless steel are good, which guarantees the precision requirements. On the other hand, the material has very small impurity release to the gas. As a gas sample cavity, the stainless steel material has good stability under the action of high and low temperatures required for pretreatment, and can cooperate with direct electric heating. The arrangement of the passivation layer further improves the stability of the tube body 100, effectively avoiding the pollution of the tube body 100 to the gas sample.

[0027] At least the surface of the temperature control section 101 is provided with a ceramic layer 120 attached thereto. The ceramic layer 120 is used to form insulation on part of the surface of the tube body 100.

[0028] By setting the ceramic layer 120 on the surface of the temperature control section 101, insulation is formed between the refrigeration structure 200 and the pipe body 100, avoiding the influence of electric heating on the refrigeration structure 200. This setting takes advantage of the good thermal stability of the ceramic layer 120, which can adapt to high and low temperature use environment, and has a certain rigidity. The required matching precision of the ceramic pipe is solved by the attachment method, and further provides a certain heat insulation effect for the refrigeration structure 200.

[0029] The connecting section 102 is provided with a first connecting piece 300, the first connecting piece 300 is made of polyimide material, and the pipe body 100 is connected with the external sample inlet channel through the first connecting piece 300. The first connecting piece 300 is used for connecting the pipe body 100 and the external gas sample inlet channel;

[0030] Unlike traditional stainless steel joints and PEEK joints, the joint made of polyimide material not only meets the demand of high temperature resistance, but also meets the demand of insulation. This makes the change of the pipe body 100 caused by direct electric heating of the pipe body 100 be completely blocked by the first connecting piece 300, avoiding the influence on the external gas sample input connection. Since the first connecting piece 300 has high sealing requirements, the joint made of whole polyimide material makes the sealing effect between the pipe body 100 and the external gas sample input connection stable. More importantly, the polyimide material can effectively control the pollution to the gas sample and the precipitation of its own substances, and its performance is stable. The first connecting piece 300 made of polyimide material is also a breakthrough in the use of mass spectrometer.

[0031] As shown in Figure 3 The electric heating section 103 and the temperature control section 101 are provided with a clamping section 104, and the clamping section 104 is provided with a second connecting piece 400; the refrigeration structure 200 layer includes a copper pipe 210 sleeved outside the temperature control section 101 and a refrigeration capillary pipe arranged on the copper pipe 210; one end of the second connecting piece 400 is connected with the copper pipe 210, and the other end is connected with the clamping section 104, so that the pipe body 100 and the copper pipe 210 are provided with an annular separation space 500 separating the pipe body 100 and the copper pipe 210. The clamping section 104 is used for clamping the second connecting piece 400, the refrigeration capillary pipe is used for cooling the temperature control section 101, the copper pipe 210 is used for forming temperature conduction and installing the refrigeration capillary pipe, the second connecting piece 400 is used for preventing the direct contact between the refrigeration structure 200 and the pipe body 100, and the annular separation space 500 is used for improving the cooperation between the pipe body 100 and the refrigeration structure 200.

[0032] The refrigeration structure 200 sleeved outside the pipe body 100 can quickly cool the pipe body 100 in a wide range, improving the refrigeration efficiency; the cooperation of the refrigeration capillary and the copper pipe 210 makes the low-temperature acting surface larger, and the structure is simple and the conductivity is good. The refrigeration structure 200 is fixed on the surface of the pipe body 100 through the second connecting piece 400, which helps to isolate the damage of the high-thermal-conductivity pipe body 100 to the copper pipe 210 and the refrigeration capillary, and plays an insulating and heat-insulating role. The setting of the annular separation space not only reduces the influence of the heat generated by the pipe body 100 on the refrigeration structure 200, but also provides a tolerance interval for the processing size error of the pipe body 100. Through the annular separation space 500, the cooperation problem caused by the local size difference or slight bending of the pipe body 100 can be effectively avoided, so that the assembly difficulty between the refrigeration structure 200 and the pipe body 100 is reduced.

[0033] The second connecting piece 400 is made of PEEK material, the clamping section 104 is provided with a high-temperature-resistant heat-resistant layer 410, and the second connecting piece 400 is connected with the clamping section 104 through the high-temperature-resistant heat-resistant layer.

[0034] The use of PEEK material helps to reduce the cost, and the high-temperature-resistant heat-resistant layer 410 is used to isolate the influence of the high temperature of the pipe body 100 on the second connecting piece 400;

[0035] Unlike traditional heating design, the refrigeration structure 200 will be affected by electricity and heat under the condition of power heating of the pipe body 100. Although the polyimide material joint can solve the two problems at the same time, the cost of the polyimide material is relatively high. Since the function of the second connecting piece 400 is to fix the refrigeration structure 200, the demand for sealing is reduced. The connecting piece made of PEEK material meets the demand for insulation, and the design of the high-temperature-resistant heat-resistant layer 410 meets the demand for heat insulation. The combination of the two can greatly reduce the cost and meet the demand for actual use.

[0036] The annular separation space 500 extends into the second connecting piece 400 and is connected with one end of the high-temperature-resistant heat-resistant layer 410 close to the temperature control section 101; the other end of the high-temperature-resistant heat-resistant layer 410 extends out of the other end of the second connecting piece 400 away from the temperature control section 101.

[0037] The annular separation space 500 extends into the second connecting piece 400, ensuring complete separation of the copper pipe 210 and the pipe body 100, and improving safety during use; and the high-temperature-resistant heat-resistant layer 410 will deform when clamping the pipe body 100 in the second connecting piece 400. Extending out of the second connecting piece 400 causes the high-temperature-resistant heat-resistant layer 410 to have different sizes inside and outside the second connecting piece 400, thereby preventing the second connecting piece 400 from moving along the axial sides while being clamped, and increasing the fixing effect on the second connecting piece 400 and the refrigeration structure 200.

[0038] The ceramic layer 120 extends to the clamping section 104 and protrudes from the side of the high-temperature-resistant heat-resistant layer 410 away from the temperature control section 101, the thickness of the ceramic layer 120 is less than the high-temperature-resistant heat-resistant layer 410, and the thickness of the annular separation space 500 is 0.5% to 1% of the length of the pipe body 100.

[0039] The extension of the ceramic layer 120 in combination with the high-temperature-resistant heat-resistant layer 410 forms better heat insulation and insulation effect on the second connecting piece 400, and the thickness limitation of the ceramic layer 120 and the thickness limitation of the annular separation space 500 help to control the overall volume on the one hand, and reduce heat loss during heating on the other hand, and are also important conditions to ensure refrigeration effect. The limitation of the two produces good cooperation effect between each other.

[0040] Embodiment 2

[0041] The embodiment is a mass spectrometer gas sample pretreatment device, which comprises a pipe body 100, a gas passage 110 is arranged in the pipe body 100, a temperature control section 101 is arranged in the middle of the pipe body 100, and connecting sections 102 are arranged at both ends of the temperature control section 101; an electrically conductive section 103 exposed outside the pipe body 100 is arranged between the connecting section 102 and the temperature control section 101, the electrically conductive section 103 is used for connecting an external power supply to the pipe body 100 to make the pipe body 100 heat up; and a refrigeration structure 200 is arranged on the surface of the temperature control section 101. The pipe body 100 is used for containing a gas sample; the temperature control section 101 is used for heating the gas sample to a high temperature and condensing and extracting a detection object at an ultra-low temperature through the pipe body 100; the connecting section 102 is used for connecting the pipe body 100 with a pipeline for conveying an external gas sample; the electrically conductive section 103 is used for connecting an external power supply to the pipe body 100 to make the pipe body 100 heat up; and the refrigeration structure 200 is used for refrigerating the temperature control section 101. The pipe body 100 can be a straight circular pipe, the length of the pipe body 100 is about 300 mm to 350 mm, the inner diameter of the pipe body 100 is about 1 mm-2 mm, and the outer diameter of the pipe body 100 is about 3 mm to 4 mm.

[0042] After the gas sample enters the tube body 100, it stays in the tube body 100, and the tube body 100 is rapidly heated by direct power supply, and the temperature rising speed can reach 50℃ / s. After the temperature rises to the specified temperature, the power supply is stopped, and the rapid cooling is performed through the refrigeration structure 200. One-time heating and cooling form one-time purging, and the temperature difference of one-time purging exceeds 400℃. After multiple purgings, the impurities in the gas sample are separated, and the part to be detected is extracted and purified and then input into the subsequent detection link. The tube body 100 is made of stainless steel, and one side of the tube body 100 for contacting the gas sample is provided with a passivation layer. The passivation layer is used to form a contact protection layer with stable structure on the inner surface of the tube body 100. The stainless steel can be 316 stainless steel. The surface of at least the temperature control section 101 is provided with a ceramic layer 120 attached. The ceramic layer 120 is used to form local insulation of the surface of the tube body 100. Specifically, the ceramic layer 120 can be a ceramic coating uniformly sprayed on the surface of the tube body 100.

[0043] The connecting section 102 is provided with a first connecting piece 300, and the first connecting piece 300 is made of polyimide. The tube body 100 is connected with the external sampling channel through the first connecting piece 300. The first connecting piece 300 is used for connecting the tube body 100 and the external gas sample input channel; the first connecting piece 300 includes a connected gas inlet channel and a connecting channel, the size of the connecting channel matches the outer diameter of the tube body 100, and the size of the gas inlet channel matches the inner diameter of the tube body 100. The gas inlet channel forms a gas inlet end at one end of the first connecting piece 300, and the connecting channel forms a connecting end at the other end of the first connecting piece 300. The surface of the first connecting piece 300 is provided with a plurality of annular grooves matched with sealing. The power supply section 103 and the temperature control section 101 are provided with a clamping section 104, and the clamping section 104 is provided with a second connecting piece 400. The refrigeration structure 200 layer includes a copper pipe 210 sleeved outside the temperature control section 101 and a refrigeration capillary pipe arranged on the copper pipe 210. One end of the second connecting piece 400 is connected with the copper pipe 210, and the other end is connected with the clamping section 104, so that the tube body 100 and the copper pipe 210 are provided with an annular separation space 500 separating the tube body 100 and the copper pipe 210.

[0044] The clamping section 104 is used for clamping the second connector 400, the refrigeration capillary is used for temperature control of the temperature control section 101, the copper pipe 210 is used for forming a temperature conduction and a refrigeration capillary installation carrier, the second connector 400 is used for preventing the refrigeration structure 200 from directly contacting the pipe body 100, and the annular separation space 500 is used for improving the cooperation between the pipe body 100 and the refrigeration structure 200. The refrigeration capillary pipe is connected with a refrigeration device outside the refrigeration capillary pipe and is wound on the surface of the copper pipe 210 to form a dense arrangement. The refrigeration capillary pipe forms a cover of the whole temperature control section 101 through the copper pipe 210, and the acting surface of the refrigeration structure 200 on the temperature control section 101 is greatly improved. The clamping section 104 is respectively arranged on both sides of the temperature control section 101, the second connector 400 is respectively arranged on both sides of the temperature control section 101, and the two ends of the copper pipe 210 are respectively connected with the temperature control section 101 but not in contact with the pipe body 100. Specifically, the second connector 400 is in threaded connection with the copper pipe 210. The center line of the pipe body 100 coincides with the center line of the copper pipe 210, and the inner diameter of the copper pipe 210 is greater than the outer diameter of the pipe body 100.

[0045] Specifically, the second connector 400 can be made of polyimide material. The second connector 400 is made of PEEK material, the clamping section 104 is provided with a high-temperature-resistant heat-resistant layer 410, and the second connector 400 is connected with the clamping section 104 through the high-temperature-resistant heat-resistant layer. The use of PEEK material helps to reduce the cost, and the high-temperature-resistant heat-resistant layer 410 is used to isolate the influence of the high temperature of the pipe body 100 on the second connector 400; the second connector 400 is sleeved on the clamping section 104, the high-temperature-resistant heat-resistant layer 410 is formed by winding high-temperature-resistant adhesive tape on the surface of the pipe body 100, one end of the second connector 400 is connected with the pipe body 100 through the high-temperature-resistant adhesive tape, and the other end is in threaded connection with the copper pipe 210. The high-temperature-resistant adhesive tape forms a tubular high-temperature-resistant heat-resistant layer 410 on the surface of the pipe body 100, and 1 / 2 to 2 / 3 of the high-temperature-resistant heat-resistant layer 410 is located in the second connector 400. The annular separation space 500 extends into the second connector 400 and is connected with one end of the high-temperature-resistant heat-resistant layer 410 close to the temperature control section 101; the other end of the high-temperature-resistant heat-resistant layer 410 extends to the other end of the second connector 400 away from the temperature control section 101.

[0046] In the second connecting piece 400, the high-temperature-resistant heat-resistant layer 410 is spaced apart from the copper pipe 210, and the annular separation space 500 extends to the outside of the copper pipe 210 and enters the interior of the second connecting piece 400. The ceramic layer 120 extends to the clamping section 104 and protrudes from the side of the high-temperature-resistant heat-resistant layer 410 away from the temperature control section 101, and the thickness of the ceramic layer 120 is less than that of the high-temperature-resistant heat-resistant layer 410. The thickness of the annular separation space 500 is 0.5% to 1% of the length of the pipe body 100. Limiting the thickness of the high-temperature-resistant heat-resistant layer 410 helps to limit the maximum distance between the copper pipe 210 and the pipe body 100, and further limits the thickness of the annular separation space 500, which is based on the length of the pipe body 100 and takes into account the processing precision required, so as to accurately control the necessary distance between the copper pipe 210 and the pipe body 100 to ensure assembly. The thickness of the annular separation space 500 is specifically the distance between the surface of the pipe body 100 and the inner surface of the copper pipe 210. In this embodiment, the ceramic layer 120 is specifically a ceramic coating sprayed on the surface of the pipe body 100. The thickness of the annular separation space 500 is 2 mm to 3 mm.

[0047] Embodiment 3

[0048] As shown in Figure 4 , this embodiment is a pretreatment system for a mass spectrometer gas sample, which comprises a gas filtering device and a temperature control system, and further comprises a pretreatment device for a mass spectrometer gas sample. The temperature control system comprises a controller and a power supply of an electrified clamp 600 connected to the controller, a refrigeration device, and a temperature measuring device. The electrified clamp 600 is connected to the electrified section 103, the refrigeration device is connected to the refrigeration structure 200, the gas filtering device is connected to the connecting section 102, and the external gas sample enters the pipe body 100 through the gas filtering device. The gas filtering device is used to dry and filter the gas sample to eliminate some interference. The temperature control system is used to collect and control the temperature of the pipe body 100. The electrified clamp 600 is used to connect the power supply to the pipe body 100. The controller is used to control the power supply and the refrigeration system. The temperature measuring device is used to collect the temperature of the pipe body 100. The pretreatment device comprises the pipe body 100, which is provided with a gas passage 110. The middle part of the pipe body 100 is provided with a temperature control section 101, and the two ends of the temperature control section 101 are provided with connecting sections 102. The connecting sections 102 and the temperature control section 101 are provided with an electrified section 103 exposed outside the pipe body 100. The electrified section 103 is used to connect to an external power supply to electrify the pipe body 100 to heat the pipe body 100. The surface of the temperature control section 101 is provided with a refrigeration structure 200.

[0049] The pipe body 100 is made of stainless steel, and one side of the pipe body 100 for contacting the gas sample is provided with a passivation layer. The surface of at least the temperature control section 101 is provided with a ceramic layer 120 attached thereto. The connecting section 102 is provided with a first connecting piece 300, and the first connecting piece 300 is made of polyimide. The pipe body 100 is connected to the external sampling channel through the first connecting piece 300. The energized section 103 is provided with a clamping section 104 between the temperature control section 101, and the clamping section 104 is provided with a second connecting piece 400. The refrigeration structure 200 layer includes a copper pipe 210 sleeved outside the temperature control section 101 and a refrigeration capillary pipe arranged on the copper pipe 210. One end of the second connecting piece 400 is connected to the copper pipe 210, and the other end is connected to the clamping section 104, so that the pipe body 100 and the copper pipe 210 are provided with an annular separation space 500 separating the pipe body 100 and the copper pipe 210. The second connecting piece 400 is made of PEEK, and the clamping section 104 is provided with a high-temperature resistant heat-resistant layer 410. The second connecting piece 400 is connected to the clamping section 104 through the high-temperature resistant heat-resistant layer. The annular separation space 500 extends into the second connecting piece 400 and is connected to the end of the high-temperature resistant heat-resistant layer 410 close to the temperature control section 101. The other end of the high-temperature resistant heat-resistant layer 410 extends to the end of the second connecting piece 400 away from the temperature control section 101.

[0050] The ceramic layer 120 extends to the clamping section 104 and protrudes from the side of the high-temperature resistant heat-resistant layer 410 away from the temperature control section 101. The thickness of the ceramic layer 120 is less than that of the high-temperature resistant heat-resistant layer 410. The thickness of the annular separation space 500 is 0.5% to 1% of the length of the pipe body 100. The electric clamp 600 is used to quickly heat the pipe body 100 under the control of the controller, greatly reducing the time required for heating in the past. At the same time, due to the simplification of the intermediate layer, the cooling speed is also greatly improved, thereby effectively reducing the time required for one cycle in the past and improving the detection efficiency. Under the action of the gas filtering device, the water and part of the conductive particles affected by ionization are filtered and adsorbed, and a relatively pure gas sample is obtained. Then, through the pretreatment device, the gas sample is purged at high temperature and adsorbed at low temperature. By utilizing the difference between the melting point and boiling point of various impurities in the gas sample and the sample to be detected, the detection object to be collected is separated, and the non-detection object is removed.

[0051] The surface of the temperature control section 101 is provided with a ceramic layer 120, and the detection end of the temperature measuring device is connected with the surface of the ceramic layer 120. The temperature measuring device is arranged on the surface of the ceramic layer 120, which helps to optimize the use environment of the temperature measuring device, thereby reducing the cost and prolonging the service life of the temperature measuring device. On the other hand, it helps to accurately measure to meet the problem of rapid heating of the conductive heating and not easy to control. Specifically, the temperature measuring device is adhered to the surface of the ceramic layer 120. The refrigeration structure 200 can be a whole machine compressor refrigeration capillary tube, which surrounds the outer layer refrigeration copper pipe 210 to refrigerate, and the outer layer refrigeration copper pipe 210 absorbs heat by cooling, and forms convection and radiation through the air in the annular separation space 500 to cool the pipe body 100 made of stainless steel. The refrigeration structure 200 is fixed on the pipe body 100 through the high-temperature resistant heat-resistant layer 410 formed by the high-temperature adhesive tape at both ends and the second connecting piece 400 formed by the PEEK sealing joint.

[0052] In actual use, one complete cycle is required for one pretreatment. First, the upper half cycle pretreatment is carried out to contact and conductively cool the pipe body 100 as a sample inlet pipe. The temperature of the pipe body 100 needs to reach a preset ultra-low temperature value, generally-160 DEG C. The temperature is maintained to continuously capture and adsorb various solid VOC components in the gas sample. After the adsorption reaches the required amount of detection material in the preset adsorption time period, the gas sample is stopped, and the oxygen and nitrogen in the pipe body 100 are removed by back blowing. Then the lower half cycle is carried out to directly heat the pipe body 100 by electrification to rapidly heat the pipe body 100, so as to rapidly gasify various solid VOCs in the pipe body 100, meet the sample inlet requirement of the rear-end testing instrument, and complete the cold-heat exchange cycle sampling device closed loop cycle. The above process is repeated to prepare the gas sample.

[0053] Obviously, the above embodiments of the present application are only examples for clearly illustrating the technical solutions of the present application, and are not intended to limit the specific embodiments of the present application. Any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A pretreatment device for gas samples in a mass spectrometer, characterized in that, The device includes a tube body, which has a gas passage. A temperature control section is located in the middle of the tube body, and connecting sections are located at both ends of the temperature control section. An exposed energized section is located between the connecting section and the temperature control section. The energized section is used to connect an external power source to energize the tube body, causing it to heat up. A cooling structure is located outside the temperature control section. At least the surface of the temperature control section of the tube body is provided with an attached ceramic layer; A clamping section is provided between the energizing section and the temperature controlling section, and a second connecting member is provided on the clamping section; The refrigeration structure includes a copper tube sleeved outside the temperature control section and a refrigeration capillary tube disposed on the copper tube; one end of the second connector is connected to the copper tube, and the other end is connected to the clamping section, so that an annular partition space is provided between the tube body and the copper tube to separate the tube body and the copper tube. The clamping section is provided with a high-temperature heat-insulating layer, and the second connector is connected to the clamping section through the high-temperature heat-insulating layer; the annular partition space extends into the second connector and is connected to one end of the high-temperature heat-insulating layer near the temperature control section, and the other end of the high-temperature heat-insulating layer extends to the outside of the end of the second connector away from the temperature control section.

2. The pretreatment device for gas samples in a mass spectrometer according to claim 1, characterized in that, The tube body is made of stainless steel, and a passivation layer is provided on the side of the tube body that is in contact with the gas sample.

3. The pretreatment device for gas samples in a mass spectrometer according to claim 1, characterized in that, The connecting section is provided with a first connector, which is made of polyimide. The tube body is connected to the external sample inlet channel through the first connector.

4. A pretreatment apparatus for a gas sample for a mass spectrometer according to any one of claims 1-3, characterized in that, The second connector is made of PEEK material.

5. The pretreatment device for a gas sample in a mass spectrometer according to claim 4, characterized in that, The ceramic layer extends to the clamping section and protrudes from the side of the high-temperature resistant heat-insulating layer away from the temperature control section. The thickness of the ceramic layer is less than that of the high-temperature resistant heat-insulating layer, and the thickness of the annular partition space is 0.5% to 1% of the tube length.

6. A pretreatment system for gas samples used in a mass spectrometer, comprising: A gas filtration device and a temperature control system, characterized in that it further includes a pretreatment device for a mass spectrometer gas sample as described in any one of claims 1-5; the temperature control system includes: The controller and the power supply, cooling device and temperature measuring device of the electric clamp connected to the controller; the electric clamp is connected to the energized section, the cooling device is connected to the cooling structure, the gas filter is connected to the connecting section, and the external gas sample enters the tube body through the gas filter.

7. The pretreatment system for gas samples in a mass spectrometer according to claim 6, characterized in that, The surface of the temperature control section is provided with a ceramic layer, and the detection end of the temperature measuring device is connected to the surface of the ceramic layer.

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