Tube and analysis system

A tube with a metal outer cylinder and fluororesin inner cylinder configuration addresses the issue of gas reactions and oxygen penetration in thermal analysis systems, enabling accurate gas analysis.

JP2026014754AActive Publication Date: 2026-01-29NETZSCH GERATEBAU GMBH
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Patent Information

Application Number
JP2024116179
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-07-09
Filing Date
2024-07-19
Publication Date
2026-01-29
Estimated Expiration
2044-07-19

AI Technical Summary

Technical Problem

Existing thermal analysis methods, such as STA-MS, face challenges in accurately analyzing gases generated during thermal decomposition due to reactions between target gases containing fluorine and capillary tubes made of glass or polytetrafluoroethylene, and oxygen penetration through PTFE tubes affecting analysis results.

Method used

A tube configuration comprising a metal outer cylinder and a fluororesin inner cylinder, with specific dimensions and materials, is used to transfer gases from thermal analysis devices to gas analyzers, preventing reactions with the inner cylinder and external oxygen penetration.

Benefits of technology

This configuration allows for accurate analysis of target gases by preventing reactions with the inner cylinder and external oxygen, ensuring reliable analysis results.

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Abstract

To provide a tube and an analysis system capable of accurately analyzing an analysis target gas discharged from a thermal analyzer or the like.SOLUTION: A tube (transfer tube 23) according to the present invention is a tube for supplying a target gas discharged from a thermal analyzer 10, a heating oven, or a heating oven-type pyrolysis device to a gas analyzing part 80, the tube including an outer cylinder part side 23a formed of a metallic material, and an inner cylinder part side 23a disposed radially inside the outer cylinder part side 23b and formed of a fluorocarbon resin.SELECTED DRAWING: Figure 1
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Description

[Technical Field]

[0001] The present disclosure relates to tubes and analytical systems. [Background technology]

[0002] Thermogravimetry (TG), which quantifies weight changes while changing the temperature of a sample, Differential Thermal Analysis (DTA), which measures the relative temperature changes of a sample against a reference substance due to phase transitions and reactions, and TG-DTA (STA, Simultaneous Thermal Analysis), which performs these simultaneously, are commonly used methods to capture weight changes associated with the thermal decomposition of a substance and to capture properties such as adsorption and desorption.

[0003] However, the above-mentioned TG and STA cannot identify gases generated due to changes in sample weight, etc. Therefore, a method (TG-MS or STA-MS) in which gases generated from a TG or STA device are introduced into a mass spectrometry (hereinafter referred to as "MS") device and MS measurements are performed in real time in synchronization with the TG or STA is known as an effective means (e.g., Non-Patent Document 1). [Prior art documents] [Non-patent literature]

[0004] [Non-Patent Document 1] Ryoichi Kinoshita and five others, "Optimization of TG / DTA-MS Measurement Conditions and Their Application to Materials Analysis," J. Mass Spectrum. Soc. Jpn, 1998, Vol. 46, No. 4, p. 365 Summary of the Invention [Problem to be solved by the invention]

[0005] In the STA-MS disclosed in Non-Patent Document 1 (for example, the one shown in FIG. 1), the target gas generated in the STA is supplied to a mass spectrometer via a capillary tube made of glass, for example. However, when the target gas contains fluorine, the target gas reacts with the capillary tube, making it impossible to perform mass analysis accurately. Furthermore, when polytetrafluoroethylene (PTFE) or the like is used for the capillary tube, the reaction with the target gas containing fluorine can be suppressed, but oxygen can penetrate the PTFE capillary tube from the outside, causing the target gas to react with oxygen. Therefore, there is still room for improvement in these respects.

[0006] In view of the above, an object of the present disclosure is to provide a tube and an analysis system that can accurately analyze a target gas for analysis discharged from a thermal analysis device or the like. [Means for solving the problem]

[0007] In order to solve the above problems, the tube according to the present disclosure comprises: [1] A tube for supplying a gas to be analyzed discharged from a thermal analyzer, a heating furnace, or a heating furnace-type pyrolysis apparatus to a gas analyzer, an outer cylinder portion formed of metal; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; The present invention is characterized by comprising:

[0008] In addition, the tube according to the present disclosure is [2] In the above configuration [1], it is preferable that the inner cylindrical portion contains at least one of polytetrafluoroethylene, modified polytetrafluoroethylene, perfluoroalkoxyalkane, ethylene-tetrafluoroethylene copolymer, perfluoroethylenepropene copolymer, and polyvinylidene fluoride.

[0009] In addition, the tube according to the present disclosure is [3] In the configuration [1] or [2] above, the outer tubular portion preferably includes at least one of stainless steel, copper, and aluminum.

[0010] In addition, the tube according to the present disclosure is [4] In the configuration described in any one of the above [1] to [3], it is preferable that the diameter of the inner surface of the outer cylindrical portion is 2 millimeters or less.

[0011] In addition, the tube according to the present disclosure is [5] In the configuration described in any one of [1] to [4] above, it is preferable that the length in the longitudinal direction is 50 centimeters or more.

[0012] In addition, the tube according to the present disclosure is [6] In the configuration described in any one of [1] to [5] above, it is preferable that the diameter of the inner surface of the inner cylindrical portion is 0.8 mm or less.

[0013] In addition, the tube according to the present disclosure is [7] In the configuration described in any one of the above [1] to [6], it is preferable that a space to which an inert gas can be supplied from the outside is provided between the inner cylindrical portion and the outer cylindrical portion.

[0014] In order to solve the above problems, the analysis system according to the present disclosure includes: [8] a thermal analysis device, a heating furnace, or a heating furnace-type pyrolysis device; a gas analysis unit that analyzes the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device; a tube for supplying the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device to the gas analysis unit; An analysis system comprising: The tube an outer cylinder portion formed of metal; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; The present invention is characterized by comprising:

[0015] In addition, the analysis system according to the present disclosure includes: [9] In the configuration described in [8] above, it is preferable that an inert gas is supplied from the outside to the space between the inner cylindrical portion and the outer cylindrical portion.

[0016] In order to solve the above problems, the analysis system according to the present disclosure includes:

[10] a thermal analysis device, a heating furnace, or a heating furnace-type pyrolysis device; a gas analysis unit that analyzes the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device; a tube for supplying the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device to the gas analysis unit; An analysis system comprising: The tube A cylindrical outer cylinder portion; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; Equipped with The space between the inner and outer cylindrical portions is supplied with an inert gas from the outside. [Effects of the Invention]

[0017] According to the present disclosure, it is possible to provide a tube and an analysis system capable of accurately analyzing a gas to be analyzed discharged from a thermal analysis device or the like. [Brief explanation of the drawings]

[0018] [Figure 1] 1 is a diagram illustrating a configuration of an analysis system according to a first embodiment of the present disclosure. [Figure 2] FIG. 2 is a cross-sectional view taken along the line AA in FIG. [Figure 3] FIG. 10 is a diagram illustrating a configuration of an analysis system according to a second embodiment of the present disclosure. [Figure 4] FIG. 10 is a diagram illustrating a configuration of an analysis system according to a third embodiment of the present disclosure. [Figure 5] FIG. 5 is a cross-sectional view taken along line BB in FIG. 4. [Figure 6] FIG. 5 is a detailed view of part C in FIG. 4. [Figure 7] FIG. 5 is an enlarged view of the thermal analysis device and the heating adapter portion in FIG. 4. DETAILED DESCRIPTION OF THE INVENTION

[0019] Hereinafter, embodiments of the present disclosure will be described in detail with reference to the drawings.

[0020] 1 is a diagram showing the configuration of an analysis system 100 according to a first embodiment of the present disclosure. The analysis system 100 according to this embodiment includes a thermal analysis device 10 such as a TG device, a gas analysis unit 80 for performing mass analysis or the like on a target gas for analysis generated and discharged by thermal analysis in the thermal analysis device 10, a gas transfer unit 20 including a transfer tube 23 (tube) for transferring the target gas for analysis discharged from the thermal analysis device 10 to the gas analysis unit 80, and a heating unit 28 such as an oven for heating the target gas for analysis before supplying it to the gas analysis unit 80.

[0021] The thermal analyzer 10 is, for example, a TG instrument, which performs thermogravimetric measurements to quantify weight changes while changing the temperature of a sample. As shown in Fig. 1, the thermal analyzer 10 heats a sample placed in a sample container 11 and a reference substance placed in a sample container 12 using a heater 15 in a heating furnace 14, and measures the weight difference between the sample and the reference substance using an electromagnetic electronic balance, thereby measuring the sample temperature and sample weight changes. An exhaust port 16 is provided at the top end of the heating furnace 14, and the gas to be analyzed, which is generated from the sample by heating, is supplied from this exhaust port 16 to a gas analysis unit 80 via a transfer tube 23 of a gas transfer unit 20.

[0022] In this embodiment, the gas generated by thermogravimetry in the thermal analysis device 10 (TG device) is transferred as the analysis target gas to the gas analysis section 80 via the transfer tube 23, but this is not limited to this configuration. The thermal analysis device 10 may be, for example, a differential thermal analysis (DTA) or DSC (differential scanning calorimeter) other than the TG device, or a TG-DTA (STA) that simultaneously performs TG and DTA, etc. Alternatively, instead of the thermal analysis device 10, a configuration may be adopted in which the analysis target gas generated by heating a sample using, for example, a heating furnace such as a forced convection constant temperature dryer (oven) or a heating furnace-type pyrolysis device is transferred to the gas analysis section 80 via the transfer tube 23.

[0023] 1, the gas to be analyzed generated during thermal analysis in the thermal analysis device 10 is supplied to a gas transfer unit 20 provided in the analysis system 100. The gas transfer unit 20 transfers the gas to be analyzed from the thermal analysis device 10 to the heating unit 28 while maintaining the gas at an appropriate temperature, and discharges gas that is not transferred to the heating unit 28 from an outlet 21a.

[0024] 1 shows an example of the configuration of the gas transfer unit 20. The gas transfer unit 20 includes a heating adapter 21 that receives the gas to be analyzed supplied from the thermal analysis device 10 and heats it to a predetermined temperature, a transfer tube 23 that sends the gas to be analyzed to the gas analysis unit 80 via a heating unit 28, and a heating tube 24 that covers at least a portion of the transfer tube 23 from the radially outer side and heats the transfer tube 23.

[0025] The heating adapter 21 heats the target gas to a predetermined temperature from the thermal analyzer 10. A transfer tube 23, which sends the target gas to the gas analyzer 80 via the heating unit 28, is attached to the heating adapter 21 on the side opposite the target gas inlet 21b via a first fitting 22. The first fitting 22 is, for example, a combination of a fitting body, a ferrule that forms a seal, and a fastening nut, and fixes the transfer tube 23 to the heating adapter 21 with the end of the transfer tube 23 on the thermal analyzer 10 side positioned within the inlet 21b of the heating adapter 21 and / or within the exhaust port 16 of the heating furnace 14.

[0026] As shown in the cross-sectional view of Figure 2, the transfer tube 23 includes a tubular outer cylinder 23a made of stainless steel and a tubular inner cylinder 23b made of polytetrafluoroethylene (PTFE) and disposed radially inside the outer cylinder 23a. The outer cylinder 23a and the inner cylinder 23b are disposed concentrically around a central axis O. In Figure 2, the inner surface of the outer cylinder 23a and the outer peripheral surface of the inner cylinder 23b are depicted as being in close contact with each other, but an appropriate gap may be provided to facilitate insertion of the inner cylinder 23b from the longitudinal end of the outer cylinder 23a.

[0027] In this embodiment, the radially outward direction refers to a direction away from the central axis O along a straight line that passes through the central axis O of the transfer tube 23 in Fig. 2 and is perpendicular to the central axis O, and the radially inward direction refers to a direction toward the central axis O along the straight line. In addition, the circumferential direction refers to a rotational direction around the central axis O.

[0028] Conventionally, materials such as quartz glass and stainless steel have been used for transfer tubes, but quartz can react with solutions of fluorine, phosphoric acid, alkaline compounds, or the like, or with these atmospheres. Furthermore, when stainless steel is used for the transfer tube, it can react with chlorine-based gases. On the other hand, when PTFE is used for the transfer tube, it can prevent the transfer tube from reacting with fluorine, phosphoric acid, alkaline compounds, or chlorine-based gases, but the PTFE allows oxygen from the outside to penetrate into the transfer tube, which can affect the analysis results.

[0029] In this embodiment, the transfer tube 23 includes an outer cylindrical portion 23a made of metal and an inner cylindrical portion 23b made of fluororesin. Therefore, the target gas does not react with the inner cylindrical portion 23b made of fluororesin, which can prevent the target gas from affecting the analysis results. In addition, the metal outer cylindrical portion 23a can effectively prevent external oxygen from penetrating into the transfer tube 23.

[0030] In addition, in order to easily connect the thermal analysis device 10 to the heating section 28 and / or the gas analysis section 80, the length of the transfer tube 23 in the direction of the central axis O (longitudinal direction) is preferably 50 centimeters or more, and more preferably 3 meters or more.

[0031] Furthermore, the outer cylindrical portion 23a preferably has an inner diameter of 2 millimeters or less. This configuration makes it possible to easily accommodate the inner cylindrical portion 23b, which will be described later and has an inner diameter of 0.05 millimeters or more and 0.8 millimeters or less, while ensuring the flexibility required for the transfer tube 23. This embodiment is particularly effective when the inner diameter of the outer cylindrical portion 23a is 0.8 millimeters or less. In this embodiment, the outer cylindrical portion 23a may have an outer diameter of 1 / 16 inches and an inner diameter of 0.8 millimeters. After extensive research, the inventors of the present application found that when the inner diameter of the outer cylindrical portion 23a is 0.8 millimeters or less and the length of the transfer tube 23 in the direction of the central axis O (longitudinal direction) is 50 centimeters or more, it is difficult to coat the inner surface of the stainless steel outer cylindrical portion 23a with a fluororesin such as PTFE. Therefore, it is preferable to form the transfer tube 23 by inserting a fluororesin tube into the outer cylindrical portion 23a as the inner cylindrical portion 23b, as in this embodiment. Furthermore, the diameter of the inner surface of the inner cylindrical portion 23b is preferably 0.05 mm or more and 0.8 mm or less. In this embodiment, for example, an inner cylindrical portion 23b with an outer diameter of 0.8 mm and an inner diameter of 0.3 mm can be used. With this configuration, the inner cylindrical portion 23b functions as a capillary tube, and the gas to be analyzed can be transferred by the pressure difference at the end of the transfer tube 23. Note that, in order to ensure a practical gas flow rate, the diameter of the inner surface of the inner cylindrical portion 23b is preferably 0.05 mm or more.

[0032] The fluororesin that can be used for the inner cylindrical portion 23b is not limited to polytetrafluoroethylene (PTFE), but may be other fluororesins such as modified polytetrafluoroethylene, perfluoroalkoxyalkane (PFA), ethylene-tetrafluoroethylene copolymer (ETFE), perfluoroethylenepropene copolymer (FEP), polyvinylidene fluoride (PVDF), etc. It is preferable that the inner cylindrical portion 23b contains at least one of the above-mentioned fluororesins.

[0033] The metal that can be used for the outer cylindrical portion 23a is not limited to stainless steel, but may be any of various other metals that have excellent corrosion resistance and gas barrier properties, such as copper or aluminum.

[0034] In addition, a gap may be provided between the inner surface of the outer tube portion 23a and the outer surface of the inner tube portion 23b to the extent that the inner tube portion 23b can be easily inserted into the inside of the outer tube portion 23a from the longitudinal end of the outer tube portion 23a.

[0035] In this embodiment, as shown in Fig. 1, a portion of the transfer tube 23 is covered with a heating tube 24, which makes it possible to heat the gas to be analyzed passing through the transfer tube 23. As shown in Fig. 1, the heating adapter 21 is provided with an outlet 21a, and the gas to be analyzed that has not been sucked into the transfer tube 23 is discharged from the outlet 21a.

[0036] 1, the other end of the transfer tube 23 is fixed to a gas analysis unit 80, such as a mass spectrometer, by a second joint 82 via a heating unit 28, such as an oven. The heating unit 28 is, for example, a forced convection constant temperature dryer, and can more accurately maintain the temperature of the transfer tube 23 at a predetermined temperature. This makes it possible to maintain the temperature of the target gas being transferred through the transfer tube 23 at a temperature that will prevent it from condensing before being introduced into the gas analysis unit 80.

[0037] In this embodiment, the target gas to be analyzed that is supplied to the gas analysis unit 80 via the transfer tube 23 is sucked in by the gas analysis unit 80. The remaining target gas to be analyzed that is not sucked in by the gas analysis unit 80 and the carrier gas from the thermal analysis device 10 are discharged to the outside from the outlet 21a. In this way, the target gas to be analyzed that is discharged from the thermal analysis device 10 is configured to naturally branch into the gas analysis path and the external discharge path.

[0038] Therefore, the type, flow rate, gas pressure, etc. of the carrier gas introduced into the thermal analysis device 10 can be set completely independently of the gas to be analyzed, and therefore thermal analysis in the thermal analysis device 10 can be performed under the same conditions as when not connected to the gas analysis unit 80.

[0039] The inner cylindrical portion 23b of the transfer tube 23 is a capillary tube with an inner diameter of, for example, 0.05 mm to 0.8 mm, and is capable of transferring the target gas by a pressure difference between the ends. In this embodiment, the pressure inside the heating furnace 14 of the thermal analysis device 10 is close to atmospheric pressure, while the ionization device of the gas analysis unit 80 (mass spectrometer) is a high vacuum. This pressure difference allows the target gas from the heating furnace 14 to be supplied to the gas analysis unit 80. The target gas does not necessarily need to be sent to the gas analysis unit 80 solely through the two-layered transfer tube 23; it may be connected to the gas analysis unit 80 via, for example, a valve. Even in this case, it is preferable that oxygen and the like are not transmitted from the outside through the connection with the valve, and that the connection with the valve does not contain a material that reacts with the target gas. The target gas discharged from the thermal analysis device 10 may be branched into multiple flow paths using, for example, a three-way joint and then transferred. Even in this case, at least one of the branched flow paths is connected to the gas analysis unit 80 via the two-layered transfer tube 23.

[0040] The gas analysis unit 80 (mass analyzer) performs mass analysis of the target gas supplied from the thermal analysis device 10. The gas analysis unit 80 includes an ionizer that ionizes the target gas supplied, electrodes that form an electric field, and an ion detector.

[0041] The gas analysis unit 80 is not limited to the above-mentioned mass spectrometer, and may be, for example, a gas chromatography mass spectrometer (GC / MS), a gas chromatography time-of-flight mass spectrometer (GC / TOFMS), a time-of-flight mass spectrometer (TOFMS), or a quadrupole mass spectrometer (QMS).

[0042] As described above, this embodiment provides a tube (transfer tube 23) for supplying a target gas to be analyzed discharged from the thermal analysis device 10, a heating furnace, or a furnace-type pyrolysis device to the gas analyzer 80. The tube is configured to include an outer cylindrical portion 23a made of metal and an inner cylindrical portion 23b made of fluororesin and disposed radially inside the outer cylindrical portion 23a. By adopting this configuration, the transfer tube 23 includes the outer cylindrical portion 23a made of metal and the inner cylindrical portion 23b made of fluororesin. Therefore, the target gas does not react with the inner cylindrical portion 23b made of fluororesin, thereby preventing the target gas from affecting the analysis results. Furthermore, the metal outer cylindrical portion 23a effectively prevents external oxygen from penetrating into the transfer tube 23, thereby preventing the target gas from affecting the analysis results.

[0043] In this embodiment, the inner cylindrical portion 23b is configured to contain at least one of polytetrafluoroethylene, modified polytetrafluoroethylene, perfluoroalkoxyalkane, ethylene-tetrafluoroethylene copolymer, perfluoroethylenepropene copolymer, and polyvinylidene fluoride. By employing such a configuration, these materials, which are fluororesins and have particularly excellent heat resistance, chemical resistance, and moldability into a tube, are used for the inner cylindrical portion 23b, thereby preventing the target gas from reacting with the inner cylindrical portion 23b and effectively preventing the analysis results from being affected.

[0044] In this embodiment, outer cylinder 23a is configured to include at least one of stainless steel, copper, and aluminum. By adopting such a configuration and using these materials, which are particularly corrosion-resistant and inexpensive among metals with excellent gas barrier properties, for outer cylinder 23a, it is possible to effectively prevent oxygen and the like from penetrating into transfer tube 23 from the outside and affecting the analysis results.

[0045] In this embodiment, the diameter of the inner surface of outer cylindrical portion 23a is set to 2 millimeters or less. By adopting such a configuration, it is possible to easily ensure the flexibility required for transfer tube 23 while accommodating inner cylindrical portion 23b, which has an inner diameter of 0.05 millimeters or more and 0.8 millimeters or less. Note that the diameter of the inner surface of outer cylindrical portion 23a is preferably 0.5 millimeters or more, from the viewpoint of ensuring a gap between the outer surface of inner cylindrical portion 23b and the outer surface of inner cylindrical portion 23b.

[0046] In this embodiment, the transfer tube 23 is configured to have a longitudinal length of 50 centimeters or more. By adopting such a configuration, the thermal analysis device 10 can be easily connected to the heating unit 28 and / or the gas analysis unit 80.

[0047] In this embodiment, the diameter of the inner surface of the inner cylindrical portion 23b is set to 0.8 mm or less. By adopting such a configuration, the inner cylindrical portion 23b functions as a capillary tube, and the gas to be analyzed can be transferred by the pressure difference at the end of the transfer tube 23. In order to ensure a practical gas flow rate, it is more preferable that the diameter of the inner surface of the inner cylindrical portion 23b be 0.05 mm or more.

[0048] Furthermore, the analysis system 100 according to this embodiment includes a thermal analysis device 10, a heating furnace or a furnace-type pyrolysis device, a gas analysis unit 80 that analyzes the target gas discharged from the thermal analysis device 10, the heating furnace or the furnace-type pyrolysis device, and a tube (transfer tube 23) for supplying the target gas discharged from the thermal analysis device 10, the heating furnace or the furnace-type pyrolysis device to the gas analysis unit 80. The tube is configured to include an outer cylindrical portion 23a made of metal and an inner cylindrical portion 23b made of fluororesin and disposed radially inside the outer cylindrical portion 23a. With this configuration, the transfer tube 23 includes the outer cylindrical portion 23a made of metal and the inner cylindrical portion 23b made of fluororesin, so that the target gas does not react with the inner cylindrical portion 23b made of fluororesin, thereby suppressing the analysis results of the target gas from being affected. Furthermore, the metallic outer cylinder portion 23a effectively prevents external oxygen from permeating into the transfer tube 23, thereby preventing the oxygen from affecting the analysis results of the target gas.

[0049] Next, a second embodiment of the present disclosure will be described in detail with reference to the drawings.

[0050] 3 is a diagram showing the configuration of an analysis system 200 according to a second embodiment of the present disclosure. The analysis system 200 according to this embodiment includes a thermal analysis device 10 such as a TG device, a gas analysis unit 80 for performing mass analysis or the like on the analysis target gas generated and discharged by thermal analysis in the thermal analysis device 10, and a gas transfer unit 20 including a transfer tube 23 (tube) for transferring the analysis target gas discharged from the thermal analysis device 10 to the gas analysis unit 80.

[0051] In this embodiment, compared to the first embodiment, the analysis system 200 does not include the heating unit 28, and the transfer tube 23 that transfers the gas to be analyzed has one end fixed to the heating adapter 21 by the first joint 22 and the other end fixed to the gas analysis unit 80 by the third joint 84 without passing through the heating unit 28. In this embodiment, even without passing through the heating unit 28, the gas to be analyzed can be heated to a predetermined temperature in the heating adapter 21 and the heating tube 24 and maintained at a temperature that will not condense before being introduced into the gas analysis unit 80.

[0052] Furthermore, in this embodiment, since the transfer tube 23 does not pass through the heating unit 28, the length of the transfer tube 23 can be shortened, and the intrusion of oxygen and the like from the outside can be more easily suppressed.

[0053] Next, a third embodiment of the present disclosure will be described in detail with reference to the drawings.

[0054] 4 is a diagram showing the configuration of an analysis system 300 according to a third embodiment of the present disclosure. The analysis system 300 according to this embodiment includes a thermal analysis device 10 such as a TG device, a gas analysis unit 80 for performing mass analysis or the like on the analysis target gas generated and discharged by thermal analysis in the thermal analysis device 10, a gas transfer unit 20 including a transfer tube 23 (tube) for transferring the analysis target gas discharged from the thermal analysis device 10 to the gas analysis unit 80, and a heating unit 28 such as an oven for heating the analysis target gas before supplying it to the gas analysis unit 80.

[0055] In this embodiment, as compared to the first embodiment, as shown in FIG. 5, a gap flow passage 23c through which an inert gas passes is provided between the inner surface of the outer cylindrical portion 23a and the outer peripheral surface of the inner cylindrical portion 23b. In this embodiment, the gap flow passage 23c can be formed, for example, by making the diameter of the inner surface of the outer cylindrical portion 23a larger than the diameter of the outer peripheral surface of the inner cylindrical portion 23b by a predetermined length. Alternatively, the gap flow passage 23c may be formed by providing, for example, protruding ribs that protrude radially inward from the inner surface of the outer cylindrical portion 23a or protrude radially outward from the outer peripheral surface of the inner cylindrical portion 23b and are spaced apart in the circumferential direction, thereby forcibly forming gaps between the protruding ribs in the circumferential direction and reliably forming the gap flow passage 23c. In this embodiment, to provide the gap flow passage 23c between the outer cylindrical portion 23a and the inner cylindrical portion 23b, the diameter of the inner surface of the outer cylindrical portion 23a is set larger than those of the first and second embodiments. The diameter of the inner surface of the outer cylindrical portion 23a is preferably, for example, 8 millimeters or less.

[0056] The inert gas flowing between the inner surface of the outer cylindrical portion 23a and the outer peripheral surface of the inner cylindrical portion 23b is, for example, argon gas, helium gas, or the like.

[0057] The inert gas to be flowed between the inner surface of the outer cylindrical portion 23a and the outer peripheral surface of the inner cylindrical portion 23b is supplied, for example, as shown in FIG. 6, by providing a T-shaped joint 88 having an inert gas supply port 88a upstream (on the right side in FIG. 6) of a fourth joint 86 that fixes the end of the transfer tube 23 on the gas analysis section 80 side to the gas analysis section 80.

[0058] The T-joint 88 is a tube joint having an approximately T-shape and arranged within the heating section 28 as shown in FIG. 4, and as shown in FIG. 6, is provided with a first through opening 88b and a second through opening 88c through which the transfer tube 23 through which the gas to be analyzed from the thermal analysis device 10 passes, and an inert gas supply port 88a oriented in a direction perpendicular to the transfer tube 23 and through which the inert gas from the gas supply section is supplied.

[0059] The transfer tube 23 is fixed in a state in which it passes through the first through opening 88b and the second through opening 88c. The transfer tube 23 fixed to the first through opening 88b and the second through opening 88c has a single-cylinder region 23s in the internal space N of the T-shaped joint 88, where only the outer cylinder portion 23a is removed. The inert gas supplied from the inert gas supply port 88a is supplied through this single-cylinder region 23s in the transfer tube 23 into the gap flow path 23c between the outer cylinder portion 23a and the inner cylinder portion 23b. The inner cylinder portion 23b is crimped and sealed by a ferrule 86a in the fourth joint 86 to prevent the inert gas supplied from the inert gas supply port 88a from flowing toward the gas analysis section 80.

[0060] The inert gas supplied into the gap flow path 23c between the outer cylindrical portion 23a and the inner cylindrical portion 23b through the single-cylinder region 23s passes through the inside of the heating portion 28 and the heating tube 24 and moves into the heating adapter 21. As shown in Figure 7, the outer cylindrical portion 23a of the transfer tube 23 terminates inside the heating adapter 21, and only the inner cylindrical portion 23b penetrates the heating adapter 21 and extends to the heating furnace 14 of the thermal analysis device 10.

[0061] As shown in FIGS. 4, 6, and 7, the inner cylindrical portion 23b of the transfer tube 23 is covered by the outer cylindrical portion 23a, except for the inside of the T-joint 88. An inert gas is supplied to the gap flow path 23c between the outer cylindrical portion 23a and the inner cylindrical portion 23b. The internal space N of the T-joint 88 is also filled with an inert gas supplied from the inert gas supply port 88a. Therefore, the analysis target gas discharged from the thermal analysis device 10 is supplied into the gas analysis unit 80 through the inner cylindrical portion 23b made of fluororesin and covered with the inert gas. This makes it possible to more effectively prevent external gases that affect gas analysis, such as oxygen, from penetrating into the inner cylindrical portion 23b and affecting the analysis results.

[0062] In this embodiment, an inert gas is supplied to the gap flow path 23c between the outer cylindrical portion 23a and the inner cylindrical portion 23b, and the gas to be analyzed passes through the inner cylindrical portion 23b made of fluororesin and covered with the inert gas, and is supplied into the gas analysis portion 80. Therefore, the outer cylindrical portion 23a does not necessarily need to be made of a metal material with excellent gas barrier properties, and may be made of a material other than metal.

[0063] As shown in Fig. 6, the end of the outer cylindrical portion 23a of the transfer tube 23 on the gas analysis section 80 side terminates inside the fourth joint 86. On the other hand, as shown in Fig. 4, the inner cylindrical portion 23b of the transfer tube 23 passes through the fourth joint 86 and extends into the gas analysis section 80. With this configuration, the gas to be analyzed discharged from the thermal analysis apparatus 10 passes through the inside of the inner cylindrical portion 23b and is supplied into the gas analysis section 80. Note that a diameter conversion joint can be used for the fourth joint 86 to convert the outer diameter of the outer cylindrical portion 23a to the outer diameter of the inner cylindrical portion 23b.

[0064] Although detailed illustration is omitted, the transfer tube 23 is fixed to the first through opening 88b and the second through opening 88c by combining a ferrule that seals the outer circumferential surface and a fastening nut that fixes the transfer tube 23 to the joint body. Also, the inert gas supply tube 87 (see FIG. 6) fixed within the inert gas supply port 88a oriented in a direction perpendicular to the transfer tube 23 is also fixed to the inert gas supply port 88a by combining a ferrule that seals the outer circumferential surface and a fastening nut that fixes the inert gas supply tube 87 to the joint body.

[0065] 7, in this embodiment, the outer cylindrical portion 23a of the transfer tube 23 terminates inside the heating adapter 21, and only the inner cylindrical portion 23b extends into the heating furnace 14 of the thermal analysis device 10. Then, the inert gas that passes through the gap flow path 23c of the transfer tube 23 and reaches the inside of the heating adapter 21 is discharged to the outside from the exhaust port 21a.

[0066] As described above, in this embodiment, a space is provided between the inner cylindrical portion 23b and the outer cylindrical portion 23a, into which an inert gas can be supplied from the outside. By adopting this configuration, the transfer tube 23 includes the inner cylindrical portion 23b, which is covered with an inert gas and made of a fluororesin. Therefore, the target gas does not react with the inner cylindrical portion 23b, which is made of a fluororesin, and the analysis results of the target gas can be prevented from being affected. Furthermore, by covering the inner cylindrical portion 23b with an inert gas, external oxygen is effectively prevented from penetrating into the transfer tube 23, thereby preventing the analysis results of the target gas from being affected.

[0067] Furthermore, the analysis system 300 according to this embodiment includes a thermal analysis device 10, a heating furnace, or a furnace-type pyrolysis device, a gas analysis unit 80 that analyzes a target gas discharged from the thermal analysis device 10, the heating furnace, or the furnace-type pyrolysis device, and a tube (transfer tube 23) for supplying the target gas discharged from the thermal analysis device 10, the heating furnace, or the furnace-type pyrolysis device to the gas analysis unit 80. The tube includes a cylindrical outer tube 23a and an inner tube 23b made of fluororesin and disposed radially inside the outer tube 23a. An inert gas is supplied from the outside to the space between the inner tube 23b and the outer tube 23a. With this configuration, the transfer tube 23 is covered with an inert gas and includes the inner tube 23b made of fluororesin. Therefore, the target gas does not react with the inner tube 23b made of fluororesin, thereby suppressing the analysis results of the target gas from being affected. Furthermore, by covering the inner cylindrical portion 23b with an inert gas, it is possible to effectively prevent external oxygen from permeating into the transfer tube 23, thereby preventing it from affecting the analysis results of the target gas.

[0068] Although the present disclosure has been described based on the drawings and examples, it should be noted that those skilled in the art can easily make various modifications or alterations based on the present disclosure. Therefore, it should be noted that these modifications and alterations are included in the scope of the present invention. For example, the functions included in each component, step, etc. can be rearranged so as not to be logically inconsistent, and multiple components and steps can be combined or divided into one.

[0069] For example, in this embodiment, the thermal analysis device 10 and the gas analysis unit 80 are connected by a transfer tube 23 having a two-layer structure. Even if there is a region along the way where the outer tube portion 23a is not provided, it is sufficient if the region is extremely short in the axial direction, such as the connection portion between tubes, or if gas barrier properties are ensured by means other than the outer tube portion 23a so that oxygen and the like do not penetrate into the inner tube portion 23b.

[0070] 2 and 5, the cross-sectional shape of the transfer tube 23 is not limited to the concentric circular shape, but may be other cross-sectional shapes such as a two-layer ellipse or a rectangle. The transfer tube 23 may also be made up of three or more layers, with an additional cylindrical portion on the outside or inside of the outer cylindrical portion 23a. [Explanation of symbols]

[0071] 10 Thermal analyzer 11,12 Sample container 14 Furnace 15 Heater 16 Exhaust port 20 Gas transfer section 21 Heating adapter 21a Outlet 21b Inlet 22 First joint 23 Transfer tube (tube) 23a Outer cylinder 23b Inner cylinder part 23c Gap channel 23s Mono-cylinder Range 24 Heating tube 28 Heating section 80 Gas Analysis Section 82 Second joint 84 Third joint 86 Fourth Joint 86a ferrule 87 Inert gas supply tube 88 T-joint 88a Inert gas supply port 88b 1st through opening 88c 2nd through opening 100, 200, 300 Analysis Systems N Internal space O center axis

Claims

1. A tube for supplying a gas to be analyzed discharged from a thermal analyzer, a heating furnace, or a heating furnace-type pyrolysis apparatus to a gas analyzer, an outer cylinder portion formed of metal; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; A tube comprising:

2. 2. The tube according to claim 1, wherein the inner cylindrical portion contains at least one of polytetrafluoroethylene, modified polytetrafluoroethylene, perfluoroalkoxyalkane, ethylene-tetrafluoroethylene copolymer, perfluoroethylenepropene copolymer, and polyvinylidene fluoride.

3. The tube according to claim 1 or 2, wherein the outer cylinder portion includes at least one of stainless steel, copper, and aluminum.

4. 3. The tube according to claim 1, wherein the diameter of the inner surface of the outer cylindrical portion is 2 millimeters or less.

5. 3. The tube according to claim 1, wherein the longitudinal length is 50 centimeters or more.

6. 3. The tube according to claim 1, wherein the diameter of the inner surface of the inner cylindrical portion is 0.8 mm or less.

7. 3. The tube according to claim 1, wherein a space is provided between the inner cylindrical portion and the outer cylindrical portion, into which an inert gas can be supplied from the outside.

8. a thermal analysis device, a heating furnace, or a heating furnace-type pyrolysis device; a gas analysis unit that analyzes the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device; a tube for supplying the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device to the gas analysis unit; An analysis system comprising: The tube an outer cylinder portion formed of metal; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; An analysis system comprising:

9. The analytical system according to claim 8 , wherein an inert gas is supplied from outside to the space between the inner cylindrical portion and the outer cylindrical portion.

10. a thermal analysis device, a heating furnace, or a heating furnace-type pyrolysis device; a gas analysis unit that analyzes the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device; a tube for supplying the analysis target gas discharged from the thermal analysis device, the heating furnace, or the heating furnace-type pyrolysis device to the gas analysis unit; An analysis system comprising: The tube A cylindrical outer cylinder portion; an inner cylindrical portion made of fluororesin and disposed radially inside the outer cylindrical portion; Equipped with An analytical system, wherein an inert gas is supplied from outside to a space between the inner cylindrical portion and the outer cylindrical portion.