Gas analysis device and gas analysis method

Abstract

A gas analysis apparatus and method are disclosed that can perform measurements in direct and collection modes without complex control. The gas analysis apparatus 100 according to this disclosure includes: a branching component 20 for branching a target gas; a mass spectrometer 80 for mass spectrometry analysis of one branch of the target gas; a collection component 60 for holding another branch of the target gas; a gas chromatograph 70 for analyzing the other branch of the target gas held by the collection component; and a controller 50 for controlling the flow paths of the one branch of the target gas and the other branch of the target gas. During thermal analysis, the branching component 20 is controlled to continuously branch the supplied target gas and discharge the one branch of the target gas and the other branch of the target gas, and after the thermal analysis is completed, the other branch of the target gas held by the collection component 60 is supplied to the gas chromatograph 70.

Description

[0001] This application is a divisional application of China National Intellectual Property Administration (CNIPA) application No. 202010992523.4 entitled “Gas Analysis Apparatus and Gas Analysis Method”, filed on September 21, 2020. Technical Field

[0002] This disclosure relates to a gas analysis apparatus and a gas analysis method. Background Technology

[0003] To determine weight changes associated with the thermal decomposition of a substance, or characteristics such as adsorption and desorption, commonly used techniques include: thermogravimetric analysis (hereinafter referred to as "TG"), which quantifies weight changes while altering the temperature of the sample; differential thermal analysis (hereinafter referred to as "DTA"), which measures the relative temperature change of the sample relative to a reference material in relation to a phase transition or reaction; and TG-DTA (simultaneous thermal analysis; hereinafter referred to as "STA"), which performs these measurements.

[0004] In the aforementioned TG and STA, the gas generated accompanying the weight change of the sample cannot be identified. Therefore, as an effective method, in a known method, the gas generated from the TG or STA device is introduced into a mass spectrometer (hereinafter referred to as "MS") for real-time MS measurement in TG or STA synchronization mode (via direct mode of TG-MS or STA-MS) (see, for example, Non-Patent Literature 1).

[0005] In addition, when multiple gases are generated and the analysis becomes complex, as another effective means for gas analysis, in a known and commonly used method, the generated gases are collected and, after TG or STA are completed, the collected gases are analyzed by gas chromatography-mass spectrometry (hereinafter referred to as "GC / MS"). This is usually used as another effective means for gas analysis (by the collection mode of TG-GC / MS or STA-GC / MS) (see, for example, Patent Document 1).

[0006] (Patent Documents)

[0007] Patent Document 1: JP 2596882 B2

[0008] Patent Document 2: JPH 06258285 A

[0009] (Non-patent literature)

[0010] Non-patent literature 1: KINOSHITA, R., et al., “Optimization of TG / DTA-MS Measuring Conditions and Application to Material Analysis”, J. Mass Spectrum. Soc. Jpn, 1998, Vol. 46, No. 4, p. 365.

[0011] Non-patent literature 2: SAITO, Y., “Fundamentals of Thermal Analysis”, Kyoritsu Shuppan Publishing Co., Ltd., 1990, p. 300. Summary of the Invention

[0012] (Technical issues)

[0013] In the case of TG, clarifying the direct mode of Non-Patent Document 1 and the collection mode of Patent Document 1 typically requires performing TG-MS and TG-GC / MS as independent measurements, and the two cannot be performed in a single measurement. Furthermore, each time the measurement mode is changed, the connections between TG and MS, as well as between TG and GC / MS, must be re-established.

[0014] In light of the aforementioned issues, for example, Non-Patent Document 2 discloses a structure in which measurements via TG-MS in direct mode and measurements via TG-GC / MS in collection mode are switched by a knob. However, gas chromatographs are of the packed column type, and this structure cannot be applied to gas chromatographs using capillary columns, which are superior in gas separation and have recently become mainstream.

[0015] Furthermore, Patent Document 2 discloses a gas analysis device that performs a direct mode via TG-MS and a collection mode via TG-GC / MS in a single measurement, and switches between them via a valve. However, during thermal analysis, the flow path of the gas generated from the thermal analysis device must be switched between the mass spectrometer side and the collection component side, thus leaving room for improvement.

[0016] In view of these circumstances, the object of the present invention is to provide a gas analysis apparatus and a gas analysis method capable of performing measurements in direct mode and collection mode without complex control.

[0017] (Solution)

[0018] To address the aforementioned problems, the gas analysis apparatus according to this disclosure is a gas analysis apparatus for analyzing a target gas supplied from a thermal analysis apparatus. It includes: a branching component for branching the target gas; a mass spectrometer for mass spectrometry analysis of one branch of the target gas; a collection component for holding another branch of the target gas; a gas chromatograph for analyzing the other branch of the target gas; and a controller for controlling the flow paths of the one branch of the target gas and the other branch of the target gas. During thermal analysis by the thermal analysis apparatus, the branching component continuously branches the supplied target gas and discharges both the one branch of the target gas and the other branch of the target gas. Furthermore, after the thermal analysis is completed, the other branch of the target gas held by the collection component is supplied to the gas chromatograph.

[0019] In the gas analysis apparatus according to this disclosure, having the configuration described above, preferably, the controller is configured to control, during thermal analysis, that one branch of the target gas through the branching component is supplied to the mass spectrometer, another branch of the target gas through the branching component is supplied to the collection component, and a carrier gas is supplied to the gas chromatograph; and after thermal analysis is completed, the other branch of the target gas in the collection component is supplied to the gas chromatograph and the mass spectrometer.

[0020] In the gas analysis apparatus according to this disclosure, having the structure described above, preferably, the control of the flow paths of the one branch target gas and the other branch target gas by the controller is performed by controlling a 10-port valve.

[0021] In the gas analysis apparatus according to this disclosure, having the configuration described above, preferably, the target gas is branched in the thermal analysis apparatus.

[0022] To address the aforementioned problems, the gas analysis method according to this disclosure is a gas analysis method for analyzing a target gas supplied from a thermal analysis apparatus. The gas analysis method includes: a step of continuously branching the target gas supplied from the thermal analysis apparatus during thermal analysis; a step of performing mass spectrometry analysis on one branch of the target gas during thermal analysis; a step of holding the other branch of the target gas during thermal analysis; and a step of performing gas chromatography and mass spectrometry analysis on the held other branch of the target gas after the thermal analysis is completed.

[0023] (Beneficial effects)

[0024] According to this disclosure, a gas analysis apparatus and a gas analysis method are provided that can perform measurements in direct mode and collection mode without complex control. Attached Figure Description

[0025] Figure 1 This is a schematic diagram showing the structure of a gas analysis apparatus according to an embodiment of the present disclosure; Figure 2 This is a schematic diagram showing the structure of a branch component that forms part of a gas analysis apparatus according to an embodiment of the present disclosure; Figure 3 This is a flowchart illustrating the process of performing a gas analysis method according to an embodiment of the present disclosure; Figure 4 This is a schematic diagram showing the state of the valve and airflow in the direct mode of a gas analysis apparatus according to an embodiment of the present disclosure; Figure 5 This is a schematic diagram showing the state of the valve and airflow in the collection mode of a gas analysis apparatus according to an embodiment of the present disclosure; Figure 6 This is a schematic diagram showing a first variant of a branch component forming part of a gas analysis apparatus according to an embodiment of the present disclosure; and Figure 7 This is a schematic diagram showing a second variant of a branch component that forms part of a gas analysis apparatus according to an embodiment of the present disclosure. Detailed Implementation

[0026] Embodiments of this disclosure will now be described with reference to the accompanying drawings.

[0027] Figure 1 This is a schematic diagram showing the structural configuration of a gas analysis apparatus 100 according to an embodiment of the present disclosure. The gas analysis apparatus 100 according to this embodiment includes: a branching component 20 for branching a target gas generated by thermal analysis in a thermal analysis device (e.g., TG device 10); a mass spectrometer 80 for performing mass spectrometry analysis on one branch of the target gas; a collection component 60 for holding the other branch of the target gas; a gas chromatograph 70 for separating / analyzing the other branch of the target gas held in the collection component 60; a ten-way valve 30 for controlling the flow paths of the one branch of the target gas and the other branch of the target gas; and a controller 50 for controlling the ten-way valve 30, the collection component 60, the gas chromatograph 70, the mass spectrometer 80, etc. The control used herein includes, for example, sending a measurement trigger signal to the gas chromatograph 70 and the mass spectrometer 80.

[0028] exist Figure 1 In the diagram, the dashed lines extending from controller 50 to other functional components indicate the flow of various control signals. Each control signal can be transmitted / received via wired or wireless means.

[0029] The TG apparatus 10 is a device that performs thermogravimetric analysis while changing the sample temperature to quantify weight changes. For example... Figure 2 As shown, the TG device 10 uses a heater 15 in a heating furnace 14 to heat a sample placed on a sample container 11 and a reference placed on a sample container 12, and measures the weight difference between the sample and the reference using an electromagnetic balance, thereby measuring the temperature and weight change of the sample. An outlet 16 is provided at the upper end of the heating furnace 14, and the target gas generated from the sample by heating is supplied to the gas analyzer 100 from the outlet 16.

[0030] In this embodiment, the gas analysis device 100 is described as excluding the TG device 10, but the gas analysis device 100 can be configured as a system including the TG device 10.

[0031] like Figure 1 and Figure 2 As shown, the target gas generated during thermal analysis in the TG device 10 is supplied to a branching component 20 provided in the gas analyzer 100. This branching component 20 branches the target gas from the TG device 10 into (in...) Figure 4 (represented by thick solid lines) a target gas and (in) Figure 4 Another target gas (represented by a thick dashed line in the middle).

[0032] Figure 2 An example of the structure of the branching component 20 is shown. The branching component 20 includes: a heating adapter 21 for receiving the target gas supplied from the TG device 10 and heating it at a predetermined temperature; a heat transfer tube 24 for heating the SUS capillary 23 that supplies the target gas to the mass spectrometer 80, etc.; and a tee connector 25 that branches the target gas to the mass spectrometer 80 side and the collection component 60 side. The branched target gas through the tee connector 25 is supplied to the mass spectrometer 80 side via a capillary 27 and also to the collection component 60 side via an additional SUS capillary 26.

[0033] The heating adapter 21 heats the target gas from the TG device 10 at a predetermined temperature. On the side of the heating adapter 21 facing the inlet 21b of the target gas, an SUS capillary 23 is attached via a collar 22 to deliver the target gas to the tee connector 25. The SUS capillary 23 is covered by a heat transfer tube 24, thereby enabling the heating of the target gas passing through the SUS capillary 23. Figure 2 As shown, the heating adapter 21 is equipped with an outlet 21a from which the target gas not drawn in by the SUS capillary tube 23 is discharged.

[0034] The other end of the SUS cap 23 is connected to the tee connector 25, such as Figure 2As shown. A portion of the target gas flowing into the tee fitting 25 is supplied to port a of the ten-way valve 30 via capillary tube 27 (see reference). Figure 1 Furthermore, another portion of the target gas flowing into the tee fitting 25 is supplied to port e of the ten-way valve 30 via an additional SUS capillary tube 26. Preferably, port ef of the ten-way valve 30, the collecting component 60, and port j of the ten-way valve 30 are connected, and a suction pump (not shown), such as a diaphragm pump or rotary pump, is further connected downstream because the suction from the branch component 20 to the collecting component 60 is stronger. Furthermore, preferably, a needle valve or mass flow controller (not shown) is provided between the suction pump and port j of the ten-way valve 30 because the amount of gas drawn into the collecting component 60 can be controlled, thus controlling the introduction of the appropriate amount of target gas into the collecting component 60. The tee fitting 25 is located in the oven 28 and is set to a temperature that does not cause condensation when the target gas is branched.

[0035] In this embodiment, as described above, another target gas is supplied to the collection unit 60 via an additional SUS capillary tube 26. This additional target gas is actively suction-controlled by a suction pump and a mass flow controller and supplied to the collection unit 60. The additional SUS capillary tube 26 can be a pipe with a large inner diameter and can be configured to have a structure without a suction pump and mass flow controller. A target gas supplied to the mass spectrometer 80 via capillary tube 27 is suctioned by the mass spectrometer 80, independent of the aforementioned collection suction path. Then, the residual target gas that was not suctioned into the mass spectrometer 80 and the collection unit 60, along with the carrier gas from the TG device 10, is discharged to the outside from the outlet 21a. In this way, the target gas discharged from the TG device 10 naturally branches into the mass spectrometry analysis path, the collection path, and the external discharge path.

[0036] Therefore, the carrier gas setting introduced into the TG device 10 is completely independent of the type, flow rate, and pressure of the target gas. Thus, thermal analysis in the TG device 10 can be performed by measurement as if it were not connected to the gas analysis device 100.

[0037] In addition, in order to control the dilution or increase of the target gas, the flow rate of the target gas entering the collection and suction path can be controlled by mass flow controllers or the like.

[0038] The capillary 27 is constructed of a capillary having, for example, an inner diameter of about 0.2 mm to 0.5 mm, and is capable of delivering the target gas via a pressure difference at its ends. In this embodiment, the pressure inside the furnace 14 of the TG device 10 is close to atmospheric pressure, while the ionization device of the mass spectrometer 80 is in a high vacuum. Therefore, the target gas from the furnace 14 can be supplied to the mass spectrometer 80 via this pressure difference. For example, a fused silica capillary or a SUS capillary that has undergone internal surface deactivation treatment can be used as the capillary 27. It should be noted that the target gas can be supplied to the mass spectrometer 80 not only through the capillary 27, but also through other means such as... Figure 1 The valves shown are connected to the mass spectrometer 80.

[0039] The SUS capillary 23 and the additional SUS capillary 26 are, for example, made of SUS with an outer diameter of about 1 / 16 inch or 1 / 8 inch. However, this application disclosure is not limited to this aspect, and other outer diameters and materials can be appropriately selected according to the flow rate, composition, etc. of the target gas. In addition, the SUS capillary 23 and the additional SUS capillary 26 may have different outer or inner diameters.

[0040] 30-way valve is made of Figure 1 The valve shown comprises 10 inlet / outlet ports a to j and is controlled by controller 50 to switch between connected and disconnected states between ports a to j. Figure 1 In the diagram, the solid lines connecting ports a and b, c and d, e and f, g and h, and i and j indicate the connection status of the ten-way valve 30 in direct mode. In this mode, one target gas from the three-way connector 25 is supplied to the mass spectrometer 80 for mass spectrometry analysis, while another target gas from the three-way connector 25 is supplied to and held by the collection unit 60. The dashed lines connecting ports b and c, d and e, f and g, h and i, and j and a indicate the connection status in collection mode. In this mode, after thermal analysis by the TG device 10, the other target gas held in the collection unit 60 is supplied to the gas chromatograph 70 for gas chromatography analysis, and then to the mass spectrometer 80 for mass spectrometry analysis. The controller 50 obtains information from the TG device 10 and switches and controls the connection of the ten-way valve 30 based on whether the TG device 10 is performing thermal analysis.

[0041] The controller 50 controls the ten-way valve 30, the collection component 60, the gas chromatograph 70, the mass spectrometer 80, etc. The controller 50 includes a microcomputer and includes an input / output interface, a CPU (Central Processing Unit), RAM (Random Access Memory), ROM (Read-Only Memory), etc. The CPU can execute control programs. RAM is suitable for temporary storage, such as variables and calculation results required for program execution. ROM is suitable for storing, for example, control programs.

[0042] The collection unit 60—during thermal analysis performed by the TG apparatus 10—holds an additional branch of the target gas supplied from the tee connector 25 via an additional SUS capillary tube 26. The target gas from the tee connector 25 is supplied to the collection unit 60 at a flow rate controlled by a mass flow controller and a diaphragm pump. The collection unit 60 holds the additional branch of the target gas and cools it with liquid nitrogen or the like. The collection unit 60 also includes a heater for immediately heating the target gas held therein upon completion of thermal analysis by the TG apparatus 10 and supplying it to the gas chromatograph 70.

[0043] The gas chromatograph 70 includes: an oven for vaporizing another analytical target gas carried by a carrier gas (He) from a collection unit 60; a capillary column for separating the analytical target gas into each compound; and a detector for detecting each separated compound. During gas chromatographic analysis, the oven raises the temperature of the capillary column from 40°C to 300°C at a substantially constant rate.

[0044] The mass spectrometer 80 performs mass spectrometry analysis on one branch of the target gas supplied directly from the three-way connector 25 in direct mode, or on another branch of the target gas after gas chromatography analysis. The mass spectrometer 80 includes an ion generator for ionizing the supplied target gas, electrodes for forming an electric field, and an ion detector.

[0045] The following will refer to Figures 3 to 5 Description of usage such as Figure 1 The gas analysis apparatus 100 shown performs the gas analysis method according to this embodiment.

[0046] First, the controller 50 of the gas analyzer 100 communicates with the TG device 10 to determine whether the TG device 10 is performing thermal analysis (thermogravimetric measurement) (step S101). For example, this determination is performed when the controller 50 serially communicates with the TG device 10 and obtains the current status of the TG device 10. The controller 50 can be configured to determine that thermal analysis is being performed (determined as "yes" in step S101) and continue in this direct mode until a thermal analysis end trigger signal is received from the TG device 10 in step S101.

[0047] When the controller 50 determines in step S101 that the TG device 10 is performing thermal analysis (if "Yes" is true in step S101), the controller 50 executes control to continue the direct mode state. For example, if no thermal analysis end trigger signal is received from the TG device 10, the controller 50 determines that thermal analysis is in progress (if "Yes" is true in step S101). The controller 50 causes the target gas discharged from the furnace 14 of the TG device 10 to branch at the branching member 20 (step S103). For example, the branching of the target gas can be performed by the controller 50 by controlling the supply of carrier gas to the TG device 10, so that the target gas from the TG device 10 flows to the gas analysis device 100 side.

[0048] like Figure 2 As shown, the target gas is branched in the branching member 20 by a three-way connector 25 that distributes the target gas. The target gas has been supplied through the SUS capillary tube 23 to the flow path leading to the mass spectrometer 80 and the flow path leading to the collection member 60. In other words, in this embodiment, the supplied target gas always branches at the branching member 20 and is discharged after being divided into one branch of target gas and another branch of target gas. Therefore, during thermal analysis, it is not necessary to switch the flow path of the gas generated from the TG device 10 between the mass spectrometer 80 side and the collection member 60 side. In these respects, the structure of the gas analysis apparatus 100 according to this embodiment is significantly different from the apparatus in Patent Document 2, in which the gas is supplied discontinuously during thermal analysis by alternating switching between the mass spectrometer side and the gas collection side.

[0049] In direct mode, set the ten-way valve 30 to Figure 4 In the shown configuration, branch component 20 is directly connected to mass spectrometer 80 via capillary tube 27 and ports a and b of ten-way valve 30. Therefore, a branch of the target gas is directly introduced into mass spectrometer 80 for mass spectrometry analysis (step S105). Figure 4 In the diagram, the flow of the target gas in one branch is represented by a thick solid line. The thermal analysis in the TG device 10 and the mass spectrometry analysis in the mass spectrometer 80 can be performed synchronously directly between the devices.

[0050] Simultaneously, in direct mode, another branch of the target gas in the gas to be analyzed, branched in branching component 20, is held in collecting component 60 through ports e and f of ten-way valve 30 (step S107). Furthermore, the controller 50 utilizes liquefied nitrogen to cool the other branch of the target gas supplied to collecting component 60. Figure 4 In the diagram, the flow of the other branch of the target gas is represented by a thick dashed line.

[0051] In addition, Figure 3Although the flowchart shown describes step S107 being executed after step S105, steps S103 to S107 are preferably executed in parallel. In particular, it is preferable to control the ten-way valve 30 while the necessary switching occurs between steps S105 and S107.

[0052] In addition, in direct mode, such as Figure 4 As shown, port g and port h are in fluid communication, and the He gas flowing into port h is discharged from port g and injected into the capillary column via the SUS capillary tube and the injection port of the gas chromatograph 70.

[0053] In direct mode, ports c and d, as well as ports i and j, are connected in the flow path until the thermal analysis measurement of the TG device 10 is completed. Thus, one end of the collection component 60 and the gas chromatograph 70 is open to the atmosphere.

[0054] On the other hand, if the controller 50 determines in step S101 that the TG device 10 is not performing thermal analysis (in the case of "No" in step S101), the controller 50 performs control in collection mode. For example, when a measurement end trigger signal is received from the TG device 10, the controller 50 determines in step S101 that the TG device 10 is not performing thermal analysis (in the case of "No" in step S101). The controller 50 performs gas chromatography-mass spectrometry (GC / MS) analysis on another branch of the target gas held by the collection component (step S109). Figure 5 As shown, step S109 is executed by controlling the ten-way valve 30 via controller 50 to fluidly connect ports f and g, and ports h and i. At this time, controller 50 heats the other branch of the target gas held in the collection unit 60 via a heater. Therefore, the He gas that has flowed into port h flows out from port i and is supplied to the collection unit 60. Thus, the other branch of the target gas in the collection unit 60 is heated by the heater and transferred by the He gas. The gas is supplied to the injection port of the gas chromatograph 70 via ports f and g. Simultaneously, controller 50 outputs a trigger signal to the gas chromatograph 70 to start the GC / MS.

[0055] Furthermore, in the collection mode of GC / MS, such as Figure 5 As shown, ports b and c are fluidly connected via a ten-way valve 30 for GC / MS. Figure 5 In the diagram, the flow of the target gas in another branch is represented by a thick dashed line.

[0056] In the GC / MS collection mode, ports d and e, as well as ports j and a, are further connected. Thus, one end of capillary 27 and the additional SUS capillary 26 of branch component 20 are connected to the atmosphere.

[0057] As described above, by utilizing the ten-way valve 30, the controller 50 can switch between direct-mode mass spectrometry (MS) and GC / MS of the target gas held in the collection unit 60 with only a single simple control of the ten-way valve 30. Furthermore, while performing mass spectrometry analysis in direct mode, He gas, as the carrier gas, can be continuously supplied to the capillary column of the gas chromatograph 70. Therefore, capillary column degradation is prevented, and the state of the capillary column remains stable during GC / MS execution after direct mode, allowing for immediate initiation of GC / MS.

[0058] In this embodiment, a ten-way valve 30 is used. However, it is obvious that a similar system can be obtained by combining multiple four-way, six-way, or eight-way valves and switching each valve simultaneously. Needless to say, a similar system can be obtained even using only ten ports of a valve with 12 or more ports.

[0059] Furthermore, triggered by the end of the direct mode (i.e., the end of the thermal analysis measurement of the TG device 10), the controller 50 can sequentially control the switching of the ten-way valve 30, the heating control of the collection component 60, the start-up of the GC / MS, the end of the GC / MS, and the re-switching of the ten-way valve 30 (from the collection mode to the direct mode), etc. Therefore, thermal analysis / MS / collection (direct mode) and GC / MS (collection mode) can be realized as a series of continuous automatic measurements.

[0060] In addition, by employing an automatic sampler in the TG device 10, the above-mentioned automatic measurement can be achieved for multiple samples.

[0061] After step S109, controller 50 determines whether to end gas analysis (step S111), and if gas analysis should be ended, it ends control ("Yes" in step S111). On the other hand, if it is determined that gas analysis should continue (if "No" is given in step S111), the process returns to step S101 to continue control.

[0062] It should be noted that Figure 2 The configuration of the branch component 20 shown is not limited to this aspect, and for example, it can be employed here. Figure 6 or Figure 7 The configuration shown.

[0063] Figure 6 A branch component 20A is shown as a first variant of the branch component 20. In this first variant, with... Figure 2Compared to the branch component 20 shown, the difference lies in that the capillary 27A on the TG device 10 side passes through the tee connector 25, the SUS tube 23, and the heating adapter 21, and further extends out of the inlet 21b of the heating adapter 21 to enter the furnace 14 of the TG device 10. That is, according to the first variant of the branch component 20, in direct mode, the flow path of one branch of target gas supplied to the mass spectrometer 80 and the flow path of another branch of target gas supplied to the collection component 60 are substantially branched in the furnace 14 of the TG device 10. With such a structure, the target gas from the TG device 10 can be supplied to the mass spectrometer 80 more stably in direct mode.

[0064] Figure 7 A second variant of the branching component 20, branching component 20B, is shown. This second variant differs from the first variant in that it does not use a tee connector 25. A capillary tube 27B, having one end (arranged in the furnace 14 in the same manner as in the first variant), is fixed to the heating adapter 21 by a second collar 22, different from the SUS capillary tube 23, and supplies the target gas directly to the mass spectrometer 80 via a different path than the SUS capillary tube 23. That is, also according to the second variant of the branching component 20, in direct mode, the flow path of one analytical target gas supplied to the mass spectrometer 80 and the flow path of another analytical target gas supplied to the collection component 60 are substantially branched within the furnace 14 of the TG device 10. With this structure, one branch of the target gas can be stably and directly supplied to the mass spectrometer 80 without obstructing the flow of the other analytical target gas.

[0065] It is important to note that "supplying the target gas directly to the mass spectrometer 80" does not mean that one end of the capillary extends into the mass spectrometer 80. Rather, it means that one branch of the target gas is supplied to the mass spectrometer 80 without being held at the collection unit 60 or analyzed by the gas chromatograph 70.

[0066] As described above, this embodiment provides a gas analysis apparatus 100 that analyzes a target gas supplied from a thermal analysis apparatus (TG apparatus 10). The gas analysis apparatus 100 includes: a branching component 20 that branches the target gas; a mass spectrometer 80 that performs mass spectrometry analysis on one branch of the target gas; a collection component 60 that holds the other branch of the target gas; a gas chromatograph 70 that analyzes the other branch of the target gas held by the collection component 60; and a controller 50 that controls the flow paths of the one branch of the target gas and the other branch of the target gas. During thermal analysis by the thermal analysis apparatus, the branching component 20 continuously branches the supplied target gas to discharge both the one branch of the target gas and the other branch of the target gas. When the thermal analysis is complete, the other branch of the target gas held by the collection component 60 is supplied to the gas chromatograph 70. With this structure, during thermal analysis, the target gas supplied from the TG apparatus 10 is always continuously branched by the branching component 20 and discharged towards the mass spectrometer 80 and the collection component 60. Therefore, during thermal analysis, it is not necessary to switch the flow path between the mass spectrometer 80 side and the collection component 60 side. Furthermore, since the target gas is always discharged to both the mass spectrometer 80 side and the collection component 60 side while being supplied, discontinuous supply of the target gas to the mass spectrometer 80 in direct mode is prevented. Therefore, the accuracy of mass spectrometry analysis in direct mode can be improved.

[0067] In this embodiment, the controller 50 is configured to supply one branch of the target gas through the branching component 20 to the mass spectrometer 80 and the other branch of the target gas through the branching component 20 to the collection component 60 during thermal analysis, while a carrier gas is supplied to the gas chromatograph 70. Upon completion of the thermal analysis, the target gas within the collection component 60 is supplied to the gas chromatograph 70, and the other branch of the target gas within the collection component 60 is supplied to both the gas chromatograph 70 and the mass spectrometer 80. This configuration allows for the continuous supply of He gas as a carrier gas to the capillary column of the gas chromatograph 70 while performing mass spectrometry analysis in direct mode. Therefore, capillary column degradation can be prevented, and the capillary column can be stabilized during GC / MS execution after direct mode, allowing for immediate initiation of GC / MS.

[0068] Furthermore, in this embodiment, the flow control of the target gas in one branch and the target gas in the other branch by the controller 50 is configured to be performed by controlling the ten-way valve 30 by the controller 50. By adopting this configuration structure, the controller 50 can perform switching between mass spectrometry analysis in direct mode and GC / MS of the retained target gas (in collection mode) with only a simple control of the ten-way valve 30.

[0069] In this embodiment, the target gas is configured to branch within the thermal analysis apparatus (TG apparatus 10). By employing this configuration, the target gas can be supplied more stably from the TG apparatus 10 to the mass spectrometer 80 in direct mode.

[0070] Furthermore, the gas analysis method according to this embodiment is a gas analysis method for analyzing a target gas supplied from a thermal analysis apparatus (TG apparatus 10), wherein the method includes: a step of continuously branching the target gas supplied from the thermal analysis apparatus during thermal analysis; a step of performing mass spectrometry analysis on one branch of the target gas during thermal analysis; a step of holding the other branch of the target gas; and a step of performing gas chromatography and mass spectrometry analysis on the held target gas after the thermal analysis is completed. By adopting this configuration, the target gas supplied from the TG apparatus 10 is always continuously branched at the branching member 20 and discharged to the mass spectrometer 80 side and the collection member 60 side, thus eliminating the need to switch the flow path between the mass spectrometer 80 side and the collection member 60 side. In addition, since the target gas is always discharged to the mass spectrometer 80 side and the collection member 60 side while being supplied, discontinuous supply of the target gas to the mass spectrometer 80 in direct mode is prevented. Therefore, the accuracy of mass spectrometry analysis in direct mode can be improved.

[0071] Although this disclosure is described with reference to the accompanying drawings and examples, it should be noted that various changes or modifications can be readily made by those skilled in the art based on this disclosure. Therefore, it should be understood that such modifications or other variations are included within the scope of this invention. For example, the functions included in each component, each step, etc., can be rearranged, provided they are logically compatible, and multiple components, steps, etc., can be combined into one or separated.

[0072] For example, in this embodiment, TG is used as a thermal analysis apparatus, but this disclosure is not limited to this aspect. DSC, DTA, and various STAs can be used as thermal analysis apparatuses.

[0073] (Reference symbols)

[0074] 10TG device

[0075] Sample containers 11 and 12

[0076] 14 Heating Furnace

[0077] 15 Heaters

[0078] 16 discharge outlets

[0079] 20, 20A, 20B branch components

[0080] 21 Heating Adapter

[0081] 21a Discharge outlet

[0082] 21b Air Inlet

[0083] 22 rings

[0084] 23 SUS capillary tube

[0085] 24 heat transfer tubes

[0086] 25 T-connector

[0087] 26 Additional SUS capillary tubes

[0088] 27, 27A, 27B capillary tubes

[0089] 28 Oven

[0090] 30 valve

[0091] 50 controllers

[0092] 60 Collection Components

[0093] 70 Gas Chromatograph

[0094] 80 mass spectrometer

[0095] 100 Gas Analysis Apparatus.

Claims

1. A gas analysis apparatus for analyzing a target gas supplied from a thermal analysis apparatus, the gas analysis apparatus comprising: A branching component that branches the target gas; A mass spectrometer, which performs mass spectrometric analysis on a branch of target gases; A collection component that retains the target gas from another branch; A gas chromatograph, which analyzes the target gas in the other branch that is held; as well as A controller that controls the flow paths of the target gas in one branch and the target gas in the other branch; A portion of the branching component is always directly open to the external atmosphere. During thermal analysis using the thermal analysis device, the branching component continuously branches the supplied target gas and discharges one branch of target gas and the other branch of target gas; and After the thermal analysis is completed, the remaining target gas from the other branch is supplied to the gas chromatograph.

2. The gas analysis apparatus according to claim 1, characterized in that, The controller is configured to perform control, through which: During the aforementioned thermal analysis The target gas is supplied to the mass spectrometer through one branch of the branching component. The target gas from the other branch of the branch component is supplied to the collection component, and Carrier gas is supplied to the gas chromatograph. And after the thermal analysis is completed, The other branch of the target gas in the collection component is supplied to the gas chromatograph and the mass spectrometer.

3. The gas analysis apparatus according to claim 1 or 2, characterized in that, The controller controls the flow paths of the target gas in one branch and the target gas in the other branch by controlling a ten-way valve.

4. The gas analysis apparatus according to any one of claims 1 to 3, characterized in that, The target gas is branched in the thermal analysis apparatus.

5. The gas analysis apparatus according to any one of claims 1 to 4, characterized in that, It includes a unit for drawing the target gas from the branch component toward the collection component.

6. The gas analysis apparatus according to claim 5, characterized in that, It includes a unit for adjusting the flow rate of the other branch target gas flowing from the branch component to the collection component.

7. A gas analysis method for analyzing a target gas supplied from a thermal analysis apparatus, the gas analysis method comprising: During thermal analysis performed by the thermal analysis apparatus, the target gas supplied from the thermal analysis apparatus is continuously branched by a branching component; The thermal analysis includes the step of performing mass spectrometry analysis on a branch of the target gas. The step of holding the target gas from another branch during the thermal analysis; and After the thermal analysis is completed, the remaining target gas from the other branch is subjected to gas chromatography and mass spectrometry analysis. One portion of the branch component is always directly exposed to the external atmosphere.

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