Tubular furnace, equipment and mass spectrometry system

Abstract

The utility model provides a tubular furnace, equipment and a mass spectrometry system. The tubular furnace comprises a shell, a reactor and a heat preservation layer; the shell is of a hollow structure with a first inner cavity; the reactor comprises a reaction tube and a heating wire; the reaction tube is partially arranged in the first inner cavity in a penetrating manner; the heating wire is located in the first inner cavity and comprises a main heating section, and the main heating section is wound on the peripheral surface of the part, located in the first inner cavity, of the reaction tube and comprises a first spiral section and a second spiral section which are axially connected; the first spiral section is longer than the second spiral section, and the screw pitch of the first spiral section is longer than that of the second spiral section; the thermal insulation layer is arranged in the first inner cavity and covers the peripheral surface of the reactor. When the tubular furnace is applied to mass spectrometry, the state of a pyrolysis product of a substance to be detected can be maintained, so that the detection accuracy and reliability of the pyrolysis product in a mass spectrometer are improved.

Description

Technical Field

[0001] The utility model relates to the technical field of analysis and detection, in particular to a tubular furnace and equipment, and a mass spectrometry analysis system. Background Art

[0002] When using a mass spectrometer to analyze certain substances, it is necessary to pre-treat these substances in advance. Pyrolysis is a commonly used pre-treatment method, and its specific operation method is to place the substance to be detected in a high-temperature reactor for heating and decomposition. After the substance to be detected is decomposed, its pyrolysis products are transmitted to the mass spectrometer for detection. During the transmission process of the pyrolysis products, it is expected that the temperature change is as small as possible. This is because too large a temperature difference can easily cause the state of the substance to be detected to change, thereby reducing the possibility of the accuracy of the test results. Utility Model Content

[0003] In view of the above problems, the utility model provides a tubular furnace and equipment, and a mass spectrometry analysis system.

[0004] In order to achieve the above object, the utility model provides a tubular furnace, comprising:

[0005] The housing is a hollow structure having a first inner cavity;

[0006] A reactor, comprising a reaction tube and a heating wire; the reaction tube is partially inserted into the first inner cavity; the heating wire is located in the first inner cavity and comprises a main heating section, the main heating section is wound around the outer circumference of the portion of the reaction tube located in the first inner cavity, and comprises a first spiral section and a second spiral section connected axially, the length of the first spiral section is greater than that of the second spiral section, and the pitch of the first spiral section is greater than that of the second spiral section; and,

[0007] The heat-insulating layer is arranged in the first inner cavity and covers the outer peripheral surface of the reactor.

[0008] Optionally, both axial ends of the reaction tube extend to the outside of the shell;

[0009] The reactor further comprises a filter part and a three-way joint, wherein the filter part and the three-way joint are respectively connected to two axial ends of the reaction tube, and the filter part is located on a side of the second spiral section away from the first spiral section.

[0010] Optionally, the tube furnace also includes a support assembly, which includes a base, a first support member, a second support member and a third support member; the first support member is connected to the shell and the base; the second support member is connected to the three-way joint and the first support member; one end of the third support member is slidably connected to the base, and the other end is connected to the filter part, and the third support member can slide relative to the base along the arrangement direction of the three-way joint and the filter part.

[0011] Optionally, the filter unit includes a first end cap, a second end cap, a filter element and a clamp; the first end cap and the second end cap are respectively arranged on both sides of the filter element and clamp the filter element; the first end cap and the second end cap are also sealed and connected by the clamp; the second end cap is connected to the reaction tube;

[0012] The tube furnace further includes a heating portion, and the heating portion is disposed on the second end cover.

[0013] Optionally, a temperature monitoring component is further included; the temperature monitoring component includes a first temperature monitoring element; the first temperature monitoring element is partially arranged on the outer surface of the heating wire and is used to monitor the temperature of the heating wire.

[0014] Optionally, the tube furnace further comprises a sample feeding boat, the sample feeding boat comprises a handle and a boat body; the handle is a hollow structure having a second inner cavity, the boat body is connected to one end of the handle and has a containing cavity;

[0015] The temperature monitoring assembly further includes a second temperature monitoring element disposed in the second inner cavity.

[0016] Optionally, the number of the second helical segments is two, and the two second helical segments are respectively connected to two axial ends of the first helical segment.

[0017] To achieve the above-mentioned purpose, the utility model further provides a tubular furnace device, comprising a temperature control component and the tubular furnace as described above; the temperature control component is electrically connected to the heating wire.

[0018] Optionally, the temperature control component includes a control unit and a circuit structure; the control unit includes a multi-speed voltage regulator and a temperature controller, and the multi-speed voltage regulator and the temperature controller are electrically connected to the circuit structure respectively; the multi-speed voltage regulator is used to adjust the output voltage of the circuit structure; the temperature controller is provided with a current adjustment knob, and the current adjustment knob is used to adjust the output current of the circuit structure; the output end of the circuit structure is electrically connected to the heating wire.

[0019] To achieve the above objectives, the utility model also provides a mass spectrometry analysis system, comprising the aforementioned tubular furnace and mass spectrometer, wherein the mass spectrometer is connected to one end of the reaction tube located on the side of the second spiral section away from the first spiral section.

[0020] Compared with the prior art, the tubular furnace and equipment, and mass spectrometry analysis system of the utility model have the following advantages:

[0021] The aforementioned includes a shell, a reactor and a heat preservation layer; the shell is a hollow structure with a first inner cavity; the reactor includes a reaction tube and a heating wire; the reaction tube is partially inserted into the first inner cavity; the heating wire is located in the first inner cavity and includes a main heating section, the main heating section is wound around the outer circumference of the part of the reaction tube located in the first inner cavity, and includes a first spiral section and a second spiral section connected axially; the length of the first spiral section is greater than the length of the second spiral section, and the pitch of the first spiral section is greater than the pitch of the second spiral section; the heat preservation layer is arranged in the first inner cavity and coated on the outer circumference of the reactor. The tube section of the reaction tube corresponding to the first spiral section is the first tube section, and the tube section corresponding to the second spiral section is the second tube section. The reaction tube has a constant temperature zone, and the constant temperature zone is at least located in the area of ​​the first tube section close to the second tube section. When the tube furnace is used for mass spectrometry, one end of the reaction tube is used to connect to a mass spectrometer, and the mass spectrometer is located on the side of the second spiral section away from the first spiral section. The substance to be detected is pyrolyzed in the constant temperature zone of the reaction tube to obtain pyrolysis products, and the pyrolysis products flow from the constant temperature zone toward the direction close to the mass spectrometer and finally enter the mass spectrometer for analysis. Since the pitch of the first spiral segment is greater than the pitch of the second spiral segment, the temperature difference between the constant temperature zone and the part of the second tube segment that does not belong to the constant temperature zone is small, which makes the temperature change of the pyrolysis product during transmission in the reaction tube also correspondingly small, which is conducive to maintaining the state of the pyrolysis product, thereby improving the detection accuracy and reliability of the pyrolysis product in the mass spectrometer. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The accompanying drawings are used to better understand the present invention and do not constitute an improper limitation on the present invention.

[0023] Figure 1 It is a structural schematic diagram of a tube furnace provided by the utility model according to one embodiment;

[0024] Figure 2 It is a schematic structural diagram of a heating wire of a tubular furnace provided by the utility model according to an embodiment;

[0025] Figure 3This is a schematic structural diagram of a sample feeding boat of a tube furnace provided by the utility model according to an embodiment, wherein the joint is not shown in the figure;

[0026] Figure 4 is a cross-sectional view of a sample feeding boat of a tube furnace provided by the utility model according to one embodiment;

[0027] Figure 5 It is a partial structural schematic diagram of a tube furnace provided by the utility model according to one embodiment;

[0028] Figure 6 It is a schematic diagram of monitoring the temperature of different positions of the tube cavity of the reaction tube when the tube furnace provided by the utility model according to one embodiment is working. In the figure, different monitoring positions are marked with numbers 1-25, and there is no injection boat in the tube cavity of the reaction tube, and the heating wire includes two second tube sections;

[0029] Figure 7 It is a schematic diagram of the temperature curve in the main pipe section of the reaction tube when the tube furnace provided by the utility model according to one embodiment is working;

[0030] Figure 8 This is a schematic diagram of the temperature curve in the main pipe section of the reaction tube when the tube furnace in the comparative example is working;

[0031] Fig. 9 It is a structural schematic diagram of a tubular furnace assembly provided by the utility model according to one embodiment;

[0032] Fig.10 is a schematic structural diagram of a tubular furnace assembly provided by the utility model according to an embodiment. Fig.10 and Fig. 9 The observation direction is different.

[0033] [Description of reference numerals is as follows]:

[0034] 10-tube furnace, 100-shell, 200-reactor, 210-reaction tube, 220-heating wire, 221-main heating section, 221a-first spiral section, 221b-second spiral section, 230-three-way connector, 240-filter part, 341-first end cap, 242-second end cap, 243-filter element, 244-clamp, 245-connecting part, 300-insulation layer, 400-injection boat, 410 - boat body, 411 - accommodating cavity, 420 - handle, 421 - second inner cavity, 430 - coupling member, 500 - heating portion, 600 - supporting assembly, 610 - first supporting member, 611 - first supporting leg, 612 - second supporting leg, 620 - second supporting member, 630 - third supporting member, 640 - base, 650 - slider, 660 - guide mechanism, 710 - first temperature monitoring element, 20 - temperature control assembly. DETAILED DESCRIPTION

[0035] The following describes the implementation of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific implementations, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the illustrations provided in this embodiment only illustrate the basic concept of the present invention in a schematic manner, so the diagram only shows the components related to the present invention rather than drawing according to the number, shape and size of the components in the actual implementation. The type, quantity and proportion of each component in the actual implementation can be a random change, and the component layout type may also be more complicated.

[0036] In addition, each embodiment of the following description has one or more technical features, but this does not mean that the user of the present invention must implement all the technical features in any embodiment at the same time, or can only implement part or all of the technical features in different embodiments separately. In other words, under the premise of being possible to implement, those skilled in the art can selectively implement part or all of the technical features in any embodiment according to the disclosure of the present invention and according to the design specifications or implementation requirements, or selectively implement a combination of part or all of the technical features in multiple embodiments, thereby increasing the flexibility of the implementation of the present invention.

[0037] As used in this specification, the singular forms "one", "an" and "the" include plural objects, and the plural form "multiple" includes more than two objects, unless the content clearly indicates otherwise. As used in this specification, the term "or" is usually used in the sense of including "and / or", unless the content clearly indicates otherwise, and the terms "install", "connect", and "connect" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection. It can be a mechanical connection or an electrical connection. It can be directly connected or indirectly connected through an intermediate medium, and it can be the internal connection of two elements or the interaction relationship between two elements. Relational terms such as the terms "first", "second", etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations, nor do they indicate or imply relative importance or implicitly indicate the number of technical features indicated. It should be understood that for ordinary technicians in this field, the specific meanings of the above terms in the utility model can be understood according to specific circumstances.

[0038] In order to make the purpose, advantages and features of the utility model clearer, the utility model is further described in detail below in conjunction with the accompanying drawings. It should be noted that the drawings are all in a very simplified form and are not in precise proportions, and are only used to conveniently and clearly assist in explaining the purpose of the embodiments of the utility model. The same or similar reference numerals in the drawings represent the same or similar components.

[0039] Figure 1 FIG. 1 is a schematic diagram showing the structure of a tube furnace 10 provided by the present invention according to an embodiment. Figure 1 As shown, the tube furnace 10 includes a shell 100, a reactor 200 and an insulation layer 300. The shell 100 is a hollow structure having a first inner cavity (not marked in the figure). The reactor 200 includes a reaction tube 210 and a heating wire 220, wherein the reaction tube 210 is partially penetrated in the first inner cavity, the heating wire 220 is located in the first inner cavity, and includes a main heating section 221, and the main heating section 221 is spirally wound on the outer circumference of the portion of the reaction tube 210 located in the first inner cavity. The insulation layer 300 is located in the first inner cavity and is coated on the outer circumference of the reactor 200.

[0040] Figure 2 Schematic diagram of the structure of the heating wire 220. Figure 2 As shown, the main heating section 221 is formed into a three-dimensional spiral structure and includes a first spiral section 221a and a second spiral section 221b connected axially. The length of the first spiral section 221a is greater than the length of the second spiral section 221b, and the pitch L1 of the first spiral section 221a is greater than the pitch L2 of the second spiral section 221b.

[0041] The part of the reaction tube 210 located in the shell 100 is called the main tube section, the part of the main tube section corresponding to the first spiral section 221a is the first tube section (not marked in the figure), and the part of the main tube section corresponding to the second spiral section 221b is the second tube section. That is, the first spiral section 221a is sleeved on the outer circumferential surface of the first tube section, and the second spiral section 221b is sleeved on the second tube section. Therefore, the length of the first tube section is greater than the length of the second tube section, and the winding density of the heating wire 220 on the first tube section is less than the winding density on the second tube section. The advantage of this arrangement is that when the tube furnace 10 is working, the second spiral section 221b can generate more heat per unit length in its axial direction. In this way, in addition to the heat consumed by heat exchange with cold air, there is still more heat to heat the second tube section, so that the temperature rise of the second tube section is larger, thereby reducing the temperature difference between the constant temperature zone of the reaction tube 210 and the part of the second tube section that does not belong to the constant temperature zone.

[0042] The constant temperature zone of the reaction tube 210 refers to the area on the reaction tube 210 where the temperature is approximately constant when the tube furnace 10 is working. It should be understood that the temperature difference between any two points in the constant temperature zone is within a preset range. In some cases, the constant temperature zone is located at the part of the first tube segment close to the second tube segment, and the entire second tube segment does not belong to the constant temperature zone; in other cases, a part of the constant temperature zone is located at the part of the first tube segment close to the second tube segment, and the other part is located on the second tube segment, that is, the second tube segment includes an axially connected third sub-tube segment and a fourth sub-tube segment, the third sub-tube segment is closer to the first tube segment than the fourth sub-tube segment, and the constant temperature zone includes the third sub-tube segment, but does not include the fourth sub-tube segment. For the convenience of description, the following text will take the example that the constant temperature zone is only located in the area where the first pipe segment is close to the second pipe segment, and the entire second pipe segment does not belong to the constant temperature zone. However, it should be understood that those skilled in the art can modify the following description to adapt to the situation where part of the constant temperature zone is located in the area where the first pipe segment is close to the second pipe segment, and the other part is located in the area where the second pipe segment is close to the first pipe segment.

[0043] When the tubular furnace 10 provided in the embodiment of the utility model is connected to a mass spectrometer (not shown in the figure), and the tubular furnace 10 is used to pyrolyze the substance to be detected by the mass spectrometer, the temperature change of the pyrolysis product during transmission in the reaction tube 210 can be reduced, thereby improving the detection accuracy and reliability of the pyrolysis product by the mass spectrometer.

[0044] Specifically, the housing 100 is provided with two opposite mounting holes (not marked in the figure), and the two axial ends of the reaction tube 210 respectively pass through the two mounting holes and extend to the outside of the housing 100, and one end thereof is used to connect with the mass spectrometer, and the other end is used for the boat body 410 (such as the sample injection boat 400) loaded with the substance to be tested. Figure 3 and Figure 4 The end of the reaction tube 210 used for connecting with the mass spectrometer is located at a side of the second tube section away from the first tube section.

[0045] After the boat 410 enters the tube cavity of the reaction tube 210, it is in the constant temperature zone of the reaction tube 210, so that the substance to be tested can be pyrolyzed in a basically constant temperature environment and obtain pyrolysis products. After the pyrolysis products flow out of the constant temperature zone of the reaction tube 210, they pass through the second tube section, finally flow out of the reaction tube 210, and enter the mass spectrometer for detection. Since the temperature difference between the constant temperature zone of the reaction tube 210 and the second tube section in the tubular furnace 10 provided in the embodiment of the utility model is small, the temperature change of the pyrolysis products during transmission in the reaction tube 210 is also small, which is conducive to maintaining the state of the pyrolysis products.

[0046] In some embodiments, the number of the second spiral segment 221b is one, so that the portion of the first spiral segment 221a away from the second spiral segment 221b exchanges heat with the cold air, so that less heat is used to heat the end of the first pipe segment away from the second pipe segment, resulting in a smaller temperature rise at the end of the first pipe segment away from the second pipe segment. That is, in this case, the first pipe segment includes an axially connected first sub-segment and a second sub-segment, the second sub-segment is closer to the second pipe segment than the first sub-segment, and the constant temperature zone includes the second sub-segment but does not include the first sub-segment. It should be understood that the temperature of the first sub-segment gradually increases in the direction close to the second pipe segment.

[0047] In other embodiments, Figure 3 As shown, the number of the second spiral segments 221b is two, and the two second spiral segments 221b are respectively connected to the axial ends of the first spiral segment 221a. That is, the first spiral segment 221a is located between the two second spiral segments 221b, so that the first spiral segment 221a basically does not exchange heat with the cold air, and the heat generated by it is almost all used to heat the first pipe segment, which makes the temperature rise of the entire first pipe segment larger and basically constant. In other words, the constant temperature zone includes the entire first pipe segment. This can shorten the axial size of the reaction tube 210 for the use scenario requiring a longer constant temperature zone. Moreover, when the main heating section 221 includes two second spiral segments 221b, the reaction tube 210 correspondingly has two second pipe segments. When the reaction tube 210 is connected to the mass spectrometer, there is no need to distinguish the connection orientation, which is more convenient to use.

[0048] Next, other configurations of the tube furnace 10 are introduced. For the convenience of description, the end of the reaction tube 210 connected to the mass spectrometer is referred to as the first end, and the end of the reaction tube 210 away from the mass spectrometer is referred to as the second end. In the case where the heating wire 220 includes two second spiral segments 221b, any one of the two axial ends of the reaction tube 210 is the first end, and the other is the second end. In the case where the heating wire 220 includes one second spiral segment 221b, the end of the reaction tube 210 located on the side of the second spiral segment 221b away from the first spiral segment 221a is the first end.

[0049] Preferably, the reactor 200 further includes a three-way connector 230 and a filter unit 240 .

[0050] The three-way joint 230 includes a first joint portion, a second joint portion, and a third joint portion that are interconnected, wherein the first joint portion is coaxially arranged with the second joint portion. Figure 1 In the orientation shown, the first joint portion is located on the left side, the second joint portion is located on the right side, and the third joint portion is located on the upper side. The first joint portion is connected to the second end of the reaction tube 210. The second joint portion constitutes a passage for the boat body 410 to enter and exit the reaction tube 210, and is also used to connect with the injection boat 400. The third joint portion is used to connect with a carrier gas pipeline. The carrier gas pipeline is used to introduce a carrier gas into the reaction tube 210 to purge the tube cavity of the reaction tube 210, and to enable the pyrolysis product to be transmitted from the constant temperature zone of the first tube section to the second tube section, and finally flow into the mass spectrometer.

[0051] The filter unit 240 is connected to the first end of the reaction tube 210 and is connected to the mass spectrometer. In other words, the mass spectrometer is indirectly connected to the first end of the reaction tube 210 through the filter unit 240. In this way, the pyrolysis product is transmitted from the constant temperature zone of the reaction tube 210 to the second pipe section under the action of the carrier gas, and then passes through the filter unit 240 and finally enters the mass spectrometer. In this process, the filter unit 240 can filter out large particles in the pyrolysis product to prevent large particles from entering the sampling component of the mass spectrometer and causing blockage.

[0052] Preferably, if Figure 5 As shown, the tube furnace 10 further includes a heating unit 500 , which is disposed at one end of the filter unit 240 close to the reaction tube 210 and is used to heat the end of the filter unit 240 close to the reaction tube 210 .

[0053] In an optional embodiment, please continue to refer to Figure 5The filter unit 240 includes a first end cap 241, a second end cap 242 and a filter element 243. The first end cap 241 and the second element 242 are respectively provided with two sides of the filter element 243 and are connected to each other to clamp the filter element 243, and the filter element 243 is, for example, filter paper. The second end cap 242 is connected to the first end of the reaction tube 210 in any suitable manner. It should be understood that the first end cap 241 is provided with a connection portion 245 connected to the mass spectrometer.

[0054] That is, after passing through the second pipe section, the pyrolysis product passes through the area where the second end cap 242 is located, and then is filtered by the filter element 243, and then passes through the area where the first end cap 241 is located and enters the injection component of the mass spectrometer from the connecting portion 245. In addition, the first end cap 241 is also provided with an exhaust port 246 for exhausting the carrier gas.

[0055] The heating unit 500 is disposed on the second end cap 242. Thus, the heating unit 500 performs secondary heating on the unfiltered pyrolysis products through the second end cap 242, thereby reducing or even avoiding the probability of condensation of the pyrolysis products due to temperature reduction, increasing the amount of pyrolysis products passing through the filtering unit 240, and improving the detection sensitivity of the mass spectrometer. The second end cap 242 is provided with a mounting hole (not marked in the figure). The heating unit 500 is a rod-shaped structure, which is inserted into the mounting hole.

[0056] Preferably, the filter unit 240 further includes a clamp 244, which is clamped on the outer sides of the first end cover 241 and the second end cover 242, so that the first end cover 241 and the second end cover 242 are sealed and detachably connected. This has the advantage of facilitating replacement of the filter element 243.

[0057] Optionally, the tube furnace 10 further includes a support assembly 600, and the support assembly 600 is used to support the shell 100, the reactor 200 and other components. Figure 1The support assembly 600 includes a first support member 610, a second support member 620, a third support member 630 and a base 640. The first support member 610 connects the housing 100 and the base 640. In an optional embodiment, the first support member 610 includes a first support leg 611 and a second support leg 612. The first support leg 611 connects the housing 100 and the base 640, and the second support leg 612 also connects the housing 100 and the base 640. The first support leg 611 is close to the first end of the reaction tube 210, and the second support leg 612 is close to the second end of the reaction tube 210. One end of the second support member 620 is connected to the three-way joint 230, and the other end is connected to the second support leg 612. One end of the third support member 630 is connected to the filter unit 240, and the other end is connected to the base 640.

[0058] Preferably, the reaction tube 210 is detachably connected to the three-way joint 230, the housing 100 and the filter unit 240 to facilitate maintenance of the reaction tube 210. The third support member 630 is located on the side of the first support leg 611 away from the second support leg 612, and one end of the third support member 630 away from the filter unit 240 is slidably connected to the base 640 and can move relative to the base 640 along the arrangement direction of the three-way joint 230 and the filter unit 240. The advantage of such a setting is that it can provide an operating space for the disassembly and assembly of the reaction tube 210. Specifically, when the reaction tube 210 needs to be disassembled, the connection between the reaction tube 210 and the filter unit 240 can be released first, and then the third support member 630 can be moved in a direction away from the first support leg 611, so as to drive the filter unit 240 away from the reaction tube 210 and the housing 100, and then the reaction tube 210 can be pulled out on the premise of releasing the connection between the reaction tube 210 and the three-way joint 230, so that the reaction tube 210 is separated from the housing 100. It can be understood that the operation of installing the reaction tube 210 on the housing 100 also needs to be performed in a state where the filter unit 240 is away from the housing 100. Generally, after the reaction tube 210 is connected to the three-way joint 230 and the housing 100, the third support member 630 is moved in a direction close to the first support leg 611, and finally the reaction tube 210 is connected to the filter unit 240. It should be understood that the arrangement direction of the three-way joint 230 and the filter part 240 is the axial direction of the reaction tube 210 assembled on the shell 100, and is also the arrangement direction of the first support leg 611 and the second support leg 612, and is also the axial direction of the mounting hole.

[0059] In an optional embodiment, the support assembly 600 further includes a slider 650 and a guide mechanism 660, wherein the guide mechanism is disposed on the base 640 and extends along the arrangement direction of the three-way joint 230 and the filter unit 240. The guide mechanism 660 includes but is not limited to devices such as guide grooves and guide rails. The slider 650 is connected to one end of the third support member 630 away from the filter unit 240 and is slidably disposed on the guide mechanism 660 to achieve a sliding connection between the third support member 630 and the base 640.

[0060] In addition, similar to the tubular furnace in the prior art, the tubular furnace 10 provided in the embodiment of the utility model further includes a temperature monitoring component (not marked in the figure). The temperature monitoring component is used to monitor the temperature of the reactor 200 .

[0061] Please refer back to Figure 1 The temperature monitoring component at least includes a first temperature monitoring element 710 , and the first temperature monitoring element 710 is partially disposed on the heating wire 220 and is used to monitor the temperature of the heating wire 220 .

[0062] The first temperature monitoring element 710 includes a monitoring thermocouple and a protective sleeve wrapped around the outside of the monitoring thermocouple. That is, the monitoring thermocouple monitors the temperature of the protective sleeve, and the monitoring thermocouple indirectly monitors the temperature of the heating wire 220 by monitoring the presence of the protective sleeve. It can be understood that due to the presence of the protective sleeve, the temperature measured by the monitoring thermocouple is lower than the temperature of the heating wire 220.

[0063] The monitoring thermocouple may be an S-type thermocouple, and the protective cover may be made of quartz material.

[0064] Optionally, the tube furnace 10 may further include the sample injection boat 400. The sample injection boat 400 also includes a handle 420 and a connector 430. The boat body 410 is connected to one end of the handle 420 and has a receiving cavity 411 for loading the substance to be tested. The connector 430 is connected to the other end of the handle 420. When the boat body 410 enters the first inner cavity through the second joint part and the second end of the reaction tube 210 and reaches the constant temperature zone of the first tube section, the connector 430 is located outside the second joint part and can be sealed and connected to the second joint part so that the sample injection boat 400 and the reaction tube 210 remain relatively still. The connector 430 is preferably threadedly connected to the second joint part. It should also be noted that the material of the handle 420 and the boat body 410 is preferably quartz, and the two are preferably integrally formed.

[0065] In a preferred embodiment, if Figure 4As shown, the handle 420 of the injection boat 400 is a hollow structure having a second inner cavity 421. The temperature monitoring assembly further includes a second temperature monitoring element (not shown in the figure), which is used to be partially disposed in the second inner cavity 421, and can monitor the temperature of the position corresponding to the handle 420 in the reaction tube 210 when the boat body 410 is located in the tube cavity of the reaction tube 210.

[0066] Figure 6 FIG. 1 is a schematic diagram showing a case where the main heating section 221 includes two second spiral sections 221 b, and a calibration thermocouple is inserted into the tube cavity of the reaction tube 210 to monitor the temperature at different positions of the main section of the reaction tube 210 of the tube furnace 10 when the tube furnace 10 is operated at different set temperatures. The test results are shown in FIG. Figure 7 It should be noted that Figure 6 The reaction tube 210 is made of quartz, with an inner diameter of 11 mm and an outer diameter of 17 mm. There is no sample boat 400 in the reaction tube 210, and the number of monitoring positions is 25. The 25 monitoring positions are arranged at equal intervals in the axial direction of the reaction tube 210, and the distance between two adjacent monitoring positions is 10 cm. The material of the heating wire 220 is OCr 27 Al7Mo2, the carrier gas used is nitrogen, the flow rate is 1000SCCM, the pressure is 760Torr, and the calibration thermocouple is an S-type thermocouple, which enters the reaction tube 210 from the second joint.

[0067] It should be noted that the set temperature is the temperature of the portion of the protective sleeve corresponding to the first spiral segment 211a monitored by the monitoring thermocouple, which is lower than the actual temperature of the first spiral segment 221a. Figure 7 The reason is that the set temperature in is lower than the temperature of the constant temperature zone of the reaction tube 210.

[0068] The same method was used to monitor the temperature in the main section of the reaction tube when the tube furnace provided by the comparison was operated at different set temperatures. The results are shown in Figure 8 It should be understood that the difference between the tube furnace in the comparative example and the tube furnace 10 of the present invention is that the heating wire is evenly wound on the reaction tube, and the pitch of the winding is L1.

[0069] Compare Figure 7 and Figure 8It can be seen that the temperature in the main pipe section of the reaction tube 210 of the tube furnace 10 provided by the embodiment of the utility model is more uniform and the temperature variation is smaller, thereby determining that the temperature difference between the constant temperature zone of the reaction tube 210 and the second pipe section is smaller. It should be noted that the higher the set temperature, the greater the percentage of temperature change between the two ends and the middle part of the main pipe section of the reaction tube 210 of the tube furnace 10 is because the more heat the heating wire 220 generates, the higher its efficiency in heat exchange with cold air at the two ends of the main pipe section, and the more heat is lost. The carrier gas is introduced from the second end of the reaction tube 210, resulting in the temperature of the main section of the reaction tube 210 near the second end being lower than the temperature near the first end.

[0070] Furthermore, if Fig. 9 and Fig.10 As shown, the embodiment of the utility model further provides a tubular furnace device, comprising the aforementioned tubular furnace 10 and a temperature control component 20. The temperature control component 20 is at least electrically connected to the heating wire 220 to control the temperature of the heating wire 220, thereby controlling the temperature of the reaction tube 210.

[0071] In addition, the temperature control component 20 is also connected to the temperature monitoring component for communication so as to receive the temperature monitored by the temperature control monitoring component and implement closed-loop control of the tube furnace 10 based on the temperature regulation control strategy.

[0072] It can be understood that the temperature control component 20 includes a circuit structure (not shown in the figure), and the circuit structure is connected to the heating wire 220 to supply power to the heating wire 220. The temperature control component 20 also includes a control unit, and the control unit includes a multi-speed voltage regulator and a temperature controller (not marked in the figure), and the multi-speed voltage regulator and the temperature controller are electrically connected to the circuit structure respectively. Among them, the multi-speed voltage regulator is used to adjust the output voltage of the circuit structure according to the properties of the specific substance to be tested. The temperature controller is provided with a current adjustment knob. When the operator manipulates the current adjustment knob, the output current of the circuit structure can be adjusted, so that the heating speed can be controlled by controlling the output current as needed during the heating process of the reaction tube 210.

[0073] It should be noted that the specific configuration of the circuit structure can refer to the circuit structure of a tube furnace in the prior art, which will not be described in detail here. The multi-speed voltage regulator and the temperature controller can both use commercially available products.

[0074] Furthermore, the embodiment of the utility model also provides a mass spectrometry system, which includes the aforementioned tube furnace 10 and a mass spectrometer, which is connected to one end of the reaction tube 210 located on the side of the second spiral section 221b away from the first spiral section 221a.

[0075] Although the utility model is disclosed as above, it is not limited thereto. Those skilled in the art may make various modifications and variations to the utility model without departing from the spirit and scope of the utility model. Thus, if these modifications and variations of the utility model fall within the scope of the claims of the utility model and their equivalents, the utility model is also intended to include these modifications and variations.

Claims

1. A tubular furnace, characterized in that: include: The housing is a hollow structure having a first inner cavity; A reactor, comprising a reaction tube and a heating wire; The reaction tube is partially disposed in the first inner cavity; The heating wire is located in the first inner cavity and includes a main heating section, the main heating section is wound around the outer circumference of the portion of the reaction tube located in the first inner cavity, and includes a first spiral section and a second spiral section connected axially, the length of the first spiral section is greater than that of the second spiral section, and the pitch of the first spiral section is greater than that of the second spiral section; as well as, The heat-insulating layer is arranged in the first inner cavity and covers the outer peripheral surface of the reactor.

2. The tube furnace according to claim 1, characterized in that: Both axial ends of the reaction tube extend to the outside of the shell; The reactor further comprises a filter part and a three-way joint, wherein the filter part and the three-way joint are respectively connected to two axial ends of the reaction tube, and the filter part is located on a side of the second spiral section away from the first spiral section.

3. The tube furnace according to claim 2, characterized in that: The tube furnace also includes a support assembly, which includes a base, a first support member, a second support member and a third support member; the first support member is connected to the shell and the base; the second support member is connected to the three-way joint and the first support member; one end of the third support member is slidably connected to the base, and the other end is connected to the filter part, and the third support member can slide relative to the base along the arrangement direction of the three-way joint and the filter part.

4. The tube furnace according to claim 2, characterized in that: The filter unit includes a first end cap, a second end cap, a filter element and a clamp; the first end cap and the second end cap are respectively arranged on both sides of the filter element and clamp the filter element; the first end cap and the second end cap are also sealed and connected by the clamp; the second end cap is connected to the reaction tube; The tube furnace further includes a heating portion, and the heating portion is disposed on the second end cover.

5. The tube furnace according to claim 1, characterized in that: It also includes a temperature monitoring component; the temperature monitoring component includes a first temperature monitoring element; the first temperature monitoring element is partially arranged on the outer surface of the heating wire and is used to monitor the temperature of the heating wire.

6. The tube furnace according to claim 5, characterized in that The tube furnace further includes a sample feeding boat, which includes a handle and a boat body; the handle is a hollow structure having a second inner cavity, and the boat body is connected to one end of the handle and has a receiving cavity; The temperature monitoring assembly further includes a second temperature monitoring element disposed in the second inner cavity.

7. The tube furnace according to any one of claims 1 to 6, characterized in that The number of the second helical segments is two, and the two second helical segments are respectively connected to two axial ends of the first helical segment.

8. A tubular furnace device, characterized in that: It comprises a temperature control component and a tubular furnace as described in any one of claims 1 to 7; the temperature control component is electrically connected to the heating wire.

9. The tube furnace equipment according to claim 8, characterized in that: The temperature control component includes a control unit and a circuit structure; the control unit includes a multi-speed voltage regulator and a temperature controller, the multi-speed voltage regulator and the temperature controller are electrically connected to the circuit structure respectively; the multi-speed voltage regulator is used to adjust the output voltage of the circuit structure; The temperature controller is provided with a current regulating knob, and the current regulating knob is used to regulate the output current of the circuit structure; the output end of the circuit structure is electrically connected to the heating wire.

10. A mass spectrometry system, characterized in that: It comprises a tube furnace and a mass spectrometer as described in any one of claims 1 to 7, wherein the mass spectrometer is connected to an end of the reaction tube located on a side of the second spiral section away from the first spiral section.

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