Sample supply device and gas chromatograph

Abstract

To provide a sample supply device and a gas chromatograph that can detect pressure inside a flow path for supplying pressurized gas into a sample container before supplying the pressurized gas into the sample container.SOLUTION: A sample supply device 12 comprises an insertion pipe 68, a pressurized gas supply unit 32, a valve 38, and a pressure sensor 44. The pressurized gas supply unit 32 is connected to the insertion pipe 68 via a flow path. The valve 38 opens and closes the flow path. The pressure sensor 44 detects pressure between the valve 38 and the insertion pipe 68 within the flow path. In the sample supply device 12, before supplying pressurized gas with the pressurized gas supply unit 32, with the valve 38 closed and the insertion pipe 68 inserted into a space 84 in a sample container 80, based on a detection signal from the pressure sensor 44, pressure inside the flow path connecting the pressurized gas supply unit 32 and the insertion pipe 68 is detected.SELECTED DRAWING: Figure 2

Description

Technical Field

[0001] The present invention relates to a sample supply device for supplying a sample gas and a gas chromatograph.

Background Art

[0002] For example, in a sample introduction device as disclosed in Patent Document 1 below, a sample in a sample container in which a space called a headspace is formed at the upper part is heated, so that a gas (sample gas) containing the components of the volatilized sample is stored in the headspace. When collecting the sample gas in a sample loop, a needle (insertion tube) is inserted into the sample container, and a pressurized gas is supplied into the headspace in the sample container through the needle. As a result, since the headspace is pressurized, the sample gas can be导出 to the sample loop by the pressure in the headspace.

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0004] In such a headspace sample introduction device, a valve is provided in the flow path connecting the supply port of the pressurized gas and the needle. When pressurizing the headspace with the pressurized gas, the valve is switched from the closed state to the open state with the needle inserted into the headspace in the sample container.

[0005] However, if the pressure of the sample gas in the headspace is high, the pressure in the flow path connecting the pressurized gas supply port and the needle, specifically the flow path between the closed valve and the needle, will increase when the needle is inserted into the headspace. If the pressure in this flow path is higher than the pressure of the pressurized gas, the sample gas may flow back through the flow path when the valve is opened. In such cases, parts of the flow path that would not normally be contaminated by the sample gas may become contaminated by the sample gas.

[0006] The present invention has been made in view of the above circumstances, and aims to provide a sample supply device and a gas chromatograph that can detect the pressure in the flow path for supplying pressurized gas into a sample container before supplying the pressurized gas into the sample container. [Means for solving the problem]

[0007] A first aspect of the present invention is a sample supply device for supplying sample gas generated in a space within a sample container due to the volatilization of a sample within the sample container to a supply destination, comprising an insertion tube, a pressurized gas supply unit, a valve, a pressure sensor, and a control unit. The insertion tube is inserted into the space within the sample container. The pressurized gas supply unit is connected to the insertion tube via a flow path and supplies pressurized gas to pressurize the space through the flow path and the insertion tube. The valve opens and closes the flow path. The pressure sensor detects the pressure between the valve and the insertion tube in the flow path. The control unit receives the detection signal from the pressure sensor. The control unit includes a pressurization processing unit, a sample delivery processing unit, a pressure detection processing unit, and a signal generation processing unit. The pressurization processing unit pressurizes the space by opening the valve and allowing pressurized gas to be supplied from the pressurized gas supply unit to the space through the flow path and the insertion tube while the insertion tube is inserted into the space. The sample extraction unit extracts the sample gas from the space based on the pressure in the space after processing by the pressurization unit. The pressure detection unit detects the pressure in the flow path based on the detection signal from the pressure sensor, before processing by the pressurization unit, with the valve closed and the insertion tube inserted into the space. The signal generation unit generates a signal based on the detection result from the pressure detection unit.

[0008] A second aspect of the present invention is a gas chromatograph comprising the sample supply device and a column as a recipient for the sample gas supplied from the sample supply device. [Effects of the Invention]

[0009] According to a first aspect of the present invention, the pressure in the channel for supplying pressurized gas into the sample container can be detected before supplying the pressurized gas into the sample container.

[0010] According to a second aspect of the present invention, the sample gas can be supplied to the column using a sample supply device that can detect the pressure in the channel for supplying the pressurized gas into the sample container before supplying the pressurized gas into the sample container. [Brief explanation of the drawing]

[0011] [Figure 1] This is a schematic diagram showing an example of the configuration of the gas chromatograph in this embodiment. [Figure 2] This is a schematic diagram showing an example of the configuration of the sample supply device of this embodiment. [Figure 3] This is a block diagram showing an example of the electrical configuration of the sample supply device of this embodiment. [Figure 4] This is a diagram illustrating the operation of the sample supply device of this embodiment. [Figure 5] This is a diagram illustrating the operation of the sample supply device of this embodiment. [Figure 6] This is a diagram illustrating the operation of the sample supply device of this embodiment. [Figure 7] This is a diagram illustrating the operation of the sample supply device of this embodiment. [Figure 8] This is a functional block diagram showing a specific example of the electrical configuration of the sample supply device of this embodiment. [Figure 9] This is a flowchart showing an example of the operation flow of the sample supply device of this embodiment. [Modes for carrying out the invention]

[0012] 1. Configuration of a gas chromatograph Figure 1 is a schematic diagram showing an example of the configuration of the gas chromatograph 10 in this embodiment. The gas chromatograph 10 includes a sample supply device 12, a column 14, a detector 16, and the like.

[0013] The sample supply device 12 is a device for supplying the sample gas to the supply destination. In the gas chromatograph 10, the supply destination for the sample gas is the column 14.

[0014] Column 14 is heated in column oven 18. Each component in the sample gas introduced into column 14 is separated in the process of passing through column 14 and detected by detector 16.

[0015] 2. Configuration of the sample supply device FIG. 2 is a schematic diagram showing an example of the configuration of sample supply device 12 of the present embodiment. Specifically, sample supply device 12 of the present embodiment is a device for supplying the sample gas generated in space 84 in sample container 80 to a supply destination by volatilizing sample 82 in sample container 80. Space 84 is a so-called headspace and is formed above sample 82 in sample container 80.

[0016] Sample supply device 12 includes a pressure control unit (APC) 30, a pressurized gas supply unit 32, a pressurized gas discharge unit 34, a first gas flow path 36, a first on-off valve 38, a first branch joint 40, a second gas flow path 42, a pressure sensor 44, a second branch joint 46, a third gas flow path 48, a second on-off valve 50, a flow control unit (AFC) 52, a carrier gas supply unit 54, a carrier gas discharge unit 56, a fourth gas flow path 58, a fifth gas flow path 60, a third branch joint 62, a sixth gas flow path 64, a seventh gas flow path 66, an insertion tube 68, a sample loop 70, a six-way valve 72, etc.

[0017] Pressure control unit 30 is connected to a carrier gas supply source (not shown) such as a gas cylinder, adjusts the pressure of the carrier gas to a constant pressure higher than atmospheric pressure, and supplies it as a pressurized gas. Note that the pressure of the pressurized gas can be set in advance.

[0018] Pressure control unit 30 includes a pressurized gas supply unit 32 and a pressurized gas discharge unit 34. Pressurized gas supply unit 32 is connected to first gas flow path 36, and pressurized gas discharge unit 34 is connected to third gas flow path 48. A pressurized gas at a constant pressure is supplied from pressurized gas supply unit 32 to first gas flow path 36. Also, the pressurized gas in third gas flow path 48 is discharged from pressurized gas discharge unit 34.

[0019] The first gas flow path 36 is a flow path in which one end is connected to the pressurized gas supply unit 32 and the other end is connected to port b of the six-way valve 72. Therefore, the pressurized gas supply unit 32 is connected to port b of the six-way valve 72 via the first gas flow path 36.

[0020] A first on / off valve 38 is provided in the first gas passage 36. The first on / off valve 38 is a general-purpose, electrically controllable valve such as a solenoid valve.

[0021] Furthermore, a first branch joint 40 is provided in the first gas flow path 36. Specifically, the first branch joint 40 is provided between the first on / off valve 38 and the six-way valve 72 of the first gas flow path 36.

[0022] The first branch joint 40 is a joint for connecting the end of another flow path to a flow path. Therefore, the first gas flow path 36 is branched by the first branch joint 40 and connected to the second gas flow path 42.

[0023] The second gas passage 42 is a passage whose one end is connected to the first gas passage 36 and whose other end is connected to the pressure sensor 44. In other words, the pressure sensor 44 is provided by branching off from the first gas passage 36, specifically from between the first on / off valve 38 and the six-way valve 72 of the first gas passage 36. For example, a piezoelectric element can be used as the pressure sensor 44. The type of pressure sensor 44 is not particularly limited as long as it can measure the gas pressure.

[0024] Furthermore, the second gas flow path 42 is provided with a second branch joint 46, similar to the first branch joint 40. As a result, the second gas flow path 42 is branched by the second branch joint 46 and connected to the third gas flow path 48.

[0025] The third gas passage 48 is a passage whose one end is connected to the second gas passage 42 and whose other end is connected to the pressurized gas discharge section 34. The third gas passage 48 is provided with a second on-off valve 50 similar to the first on-off valve 38.

[0026] The flow control unit 52, like the pressure control unit 30, is connected to a carrier gas supply source such as a gas cylinder (not shown in the diagram) and supplies carrier gas adjusted to a constant flow rate. The flow control unit 52 also maintains a constant flow rate for the split carrier gas before discharging it. The flow rate of the carrier gas can be set in advance.

[0027] The flow rate control unit 52 includes a carrier gas supply unit 54 and a carrier gas discharge unit 56. The carrier gas supply unit 54 is connected to the fourth gas flow path 58, and the carrier gas discharge unit 56 is connected to the sixth gas flow path 64. A constant flow rate of carrier gas is supplied to the fourth gas flow path 58 from the carrier gas supply unit 54. The carrier gas in the sixth gas flow path 64 is discharged from the carrier gas discharge unit 56.

[0028] The pressure control unit 30 and the flow rate control unit 52 may be omitted from the sample supply device 12. However, in this case, a separate device having the same functions as the pressure control unit 30 and the flow rate control unit 52 will be used.

[0029] The fourth gas passage 58 is a passage whose one end is connected to the carrier gas supply unit 54 and whose other end is connected to port d of the six-way valve 72. Therefore, the carrier gas supply unit 54 is connected to port d of the six-way valve 72 via the fourth gas passage 58.

[0030] The fifth gas flow path 60 is a flow path in which one end is connected to the column 14 and the other end is connected to port e of the hexagonal valve 72. Therefore, the column 14 is connected to port e of the hexagonal valve 72 via the fifth gas flow path 60.

[0031] Furthermore, the fifth gas flow path 60 is provided with a third branch joint 62, similar to the first branch joint 40. As a result, the fifth gas flow path 60 is branched by the third branch joint 62 and connected to the sixth gas flow path 64.

[0032] The sixth gas channel 64 has one end connected to the fifth gas channel 60 and the other end connected to the carrier gas discharge section 56. In other words, the column 14 is supplied with the remaining gas that has been separated in the sixth gas channel 64.

[0033] The seventh gas passage 66 is a passage whose one end is connected to the insertion tube 68 and whose other end is connected to port a of the six-way valve 72. Therefore, the insertion tube 68 is connected to port a of the six-way valve 72 via the seventh gas passage 66. The insertion tube 68 is a needle-shaped tube. In other words, the insertion tube 68 also serves as a passage.

[0034] The sample loop 70 is a flow path with a predetermined volume, one end of which is connected to port c of the hexagonal valve 72, and the other end of which is connected to port f of the hexagonal valve 72.

[0035] The six-way valve 72 has ports a to f and a valve body (not shown) having multiple grooves, with each groove connecting adjacent ports a to f. Furthermore, the six-way valve 72 can switch between connected port combinations by rotating the valve body.

[0036] The hexagonal valve 72 is switchable between a first state and a second state. When the hexagonal valve 72 is in the first state, as shown by the solid line, port f and port a are in communication, port b and port c are in communication, and port d and port e are in communication. When the hexagonal valve 72 is in the second state, as shown by the dashed line, port a and port b are in communication, port c and port d are in communication, and port e and port f are in communication.

[0037] Regarding the six-way valve 72, the switching between the first and second states is performed electrically, but it may also be done manually.

[0038] Furthermore, a sample container 80 can be set in such a sample supply device 12. The sample container 80 is pre-filled with a liquid or solid sample 82. The sample 82 volatilizes when heated. Therefore, in this case, a sample gas is generated in the space 84 inside the sample container 80.

[0039] Furthermore, since the sample container 80 is sealed by a septum 86, the generated sample gas is stored in the space 84 inside the sample container 80. The septum 86 is fixed by a cap 88. This makes it possible to pressurize the inside of the sample container 80 to a pressure greater than atmospheric pressure.

[0040] With this sample supply device 12, the pressurized gas supply unit 32 can be connected to the insertion tube 68 via a flow path including the first gas flow path 36, the sample loop 70, and the seventh gas flow path 66. The insertion tube 68 can also be inserted into the space 84 within the sample container 80 as appropriate.

[0041] Therefore, the sample supply device 12 is configured to supply pressurized gas to the space 84 inside the sample container 80 via the first gas channel 36, the sample loop 70, the seventh gas channel 66, and the insertion tube 68.

[0042] However, the sample supply device 12 may be configured to supply pressurized gas to the space 84 within the sample container 80 without passing through the sample loop 70. Also, if it is possible to supply pressurized gas to the space 84 and sample gas to the column 14, for example, multiple three-way valves may be used instead of the six-way valve 72.

[0043] In the following, the flow path connecting the pressurized gas supply unit 32 and the insertion tube 68 will be simply referred to as the "connecting flow path." The connecting flow path includes at least the first gas flow path 36 and the seventh gas flow path 66. In the sample supply device 12 configured as shown in Figure 2, the connecting flow path includes the first gas flow path 36, the sample loop 70, and the seventh gas flow path 66.

[0044] Based on these considerations, the pressurized gas supply unit 32 is connected to the insertion tube 68 via a connecting channel, and pressurized gas for pressurizing the space 84 inside the sample container 80 can be supplied to the space 84 via the connecting channel and the insertion tube 68.

[0045] Furthermore, the first on / off valve 38 can open and close the connecting passage. In addition, the pressure sensor 44 can branch off from the space between the first on / off valve 38 and the insertion pipe 68 within the connecting passage and detect the pressure between them.

[0046] The pressure sensor 44 may be installed in the seventh gas passage 66, for example, as long as it can detect the pressure between the first on / off valve 38 and the insertion pipe 68 in the connecting passage.

[0047] Figure 3 is a block diagram showing an example of the electrical configuration of the sample supply device 12 of this embodiment. In addition to the pressure sensor 44, the sample supply device 12 includes a notification unit 74, an operation reception unit 76, and a device control unit 100.

[0048] Furthermore, each of the following components, including the device control unit 100, pressure control unit 30, first on / off valve 38, pressure sensor 44, second on / off valve 50, flow rate control unit 52, six-way valve 72, notification unit 74, and operation reception unit 76, are electrically connected to each other via a circuit 78 such as a bus.

[0049] The notification unit 74 is provided to notify predetermined matters. When providing visual notification, the notification unit 74 can be a display or a light-emitting component such as a lamp. When providing auditory notification, the notification unit 74 can be a sound-producing component such as a speaker.

[0050] The operation reception unit 76 accepts any operation. The operation reception unit 76 can be an input device such as a pointing device, keyboard, touch panel, or hardware button.

[0051] The device control unit 100 is responsible for the overall control of the sample supply device 12. The device control unit 100 includes a CPU (Central Processing Unit) 102. The device control unit 100 also includes a RAM (Random Access Memory) 104 and a storage unit 106 that can be directly accessed by the CPU 102.

[0052] RAM 104 is used as the work area and buffer area for CPU 102. Non-volatile memory such as HDD (Hard Disk Drive) or SSD (Solid State Drive) is used as the storage unit 106.

[0053] The storage unit 106 stores a program (control program) for controlling the operation of the sample supply device 12, and data (execution data) required for executing the control program. The storage unit 106 may also be configured to include a RAM 104.

[0054] Although not shown in the diagram, the sample supply device 12 is also equipped with a heater for heating the sample 82 in the sample container 80, and is electrically controllable.

[0055] Furthermore, the device control unit 100 may be omitted from the sample supply device 12. However, in this case, the operation of various components related to the sample supply device 12 is controlled by the control unit responsible for the overall control of the gas chromatograph 10. In other words, in this case, the various processes described below are performed by the control unit of the gas chromatograph 10.

[0056] 3. Operation of the sample supply device In the sample supply device 12 of this embodiment, multiple processes are executed sequentially when analyzing the sample gas. The operation of the sample supply device 12 will be described below with reference to Figures 4 to 7. Figures 4 to 7 are diagrams illustrating the operation of the sample supply device 12 of this embodiment.

[0057] In this embodiment, when analyzing a sample gas, an insertion process is performed first. The insertion process involves inserting the insertion tube 68 into the space 84 inside the sample container 80. When the insertion process begins, the hexagonal valve 72 is set to the first state, and the first on / off valve 38 and the second on / off valve 50 are closed. Furthermore, once the transitions in the states of the various valves are complete, the insertion tube 68 is inserted into the space 84 inside the sample container 80.

[0058] Therefore, once the insertion process is performed, the sample supply device 12 will be in the state shown in Figure 4. In Figure 4, the sealed flow path is represented by a dashed line.

[0059] Following the insertion process, the first pressure detection process is performed while the system remains in the state shown in Figure 4. The first pressure detection process, performed before the pressurization process described later, involves detecting the pressure in the connecting flow path, specifically between the first on-off valve 38 and the insertion tube 68, based on a detection signal from the pressure sensor 44, while the first on-off valve 38 is closed and the insertion tube 68 is inserted into the space 84.

[0060] Furthermore, when the first pressure detection process is executed, a signal (reference signal) is generated based on the detection result of that first pressure detection process. Specifically, this signal indicates the pressure in the connected flow path.

[0061] Following the first pressure detection process, the first determination process is executed while the system remains in the state shown in Figure 4. The first determination process determines, based on the reference signal, whether or not there is a possibility that the sample gas will flow back into the pressurized gas supply unit 32 from the connecting channel when the first on / off valve 38 is opened by the pressurization process described later.

[0062] In the first determination process, the pressure in the connecting channel detected by the first pressure detection process is compared with a threshold value. Specifically, the pressure value at the point when the pressure in the connecting channel detected by the first pressure detection process stabilizes is compared with the pressure value of the pressurized gas supplied from the pressurized gas supply unit 32 (pressure setting value of the pressurized gas in the pressure control unit 30). However, the threshold value is not limited to the pressure value of the pressurized gas supplied from the pressurized gas supply unit 32; it may be a value obtained by multiplying the said pressure value by a coefficient, or it may be any other value. When the pressure in the connecting channel is above the threshold value, it is determined that there is a possibility of sample gas backflow. On the other hand, when the pressure in the connecting channel is below the threshold value, it is determined that there is no possibility of sample gas backflow.

[0063] If the pressure value of the pressurized gas is used as the threshold value, it is possible to reliably determine whether the sample gas flows back from the connecting channel to the pressurized gas supply unit 32. For this reason, it is preferable to use the pressure value of the pressurized gas as the threshold value. As described above, the pressure of the pressurized gas is set in advance, so it is possible to use that value as the threshold value.

[0064] In this embodiment, if it is determined that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32 from the connecting channel, the pressurization process described later is stopped. In this case, the notification unit 74 may also notify that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32. When the pressurization process is stopped, the processes that follow the pressurized gas are also stopped. That is, the remaining processes related to the supply of sample gas are stopped.

[0065] Furthermore, if it is determined that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32 from the connecting channel, instead of stopping the pressurization process described later, the notification unit 74 may notify that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32. In addition, in this case, the operation reception unit 76 or the gas chromatograph 10 may accept an operation to adjust the pressure of the pressurized gas. For example, if the operation reception unit 76 accepts an operation to adjust the pressure of the pressurized gas and the pressure of the pressurized gas increases, the first pressure detection process and the first determination process may be executed again.

[0066] In this embodiment, if there is no possibility of sample gas flowing back from the connecting channel to the pressurized gas supply unit 32, the pressurization process is performed.

[0067] The pressurization process involves opening the first on / off valve 38 while the insertion tube 68 is inserted into the space 84 of the sample container 80, as shown in Figure 4, and supplying pressurized gas from the pressurized gas supply unit 32 to the space 84 via the connecting channel and the insertion tube 68. Once the heating process is performed, the sample supply device 12 will be in the state shown in Figure 5. The channel through which the pressurized gas flows is represented by a dashed line in Figure 5.

[0068] Furthermore, the first on / off valve 38 is closed after a predetermined time has elapsed since it was opened. The pressurization process ends when the first on / off valve 38 is closed. Therefore, once the pressurization process is complete, the sample supply device 12 returns to the state shown in Figure 4.

[0069] Following the pressurization process, the second pressure detection process is executed in the state shown in Figure 4. The second pressure detection process, like the first pressure detection process, is a process that detects the pressure in the connected flow path.

[0070] Following the second pressure detection process, the second determination process is executed while the system remains in the state shown in Figure 4. The second determination process determines whether or not there is a gas leak. In the second determination process, the amount of pressure change in the connecting channel detected by the second pressure detection process is referenced. If the pressure in the connecting channel changes by more than a threshold within a predetermined time, it is determined that a gas leak has occurred. On the other hand, if the pressure in the connecting channel does not change by more than a threshold within a predetermined time, it is determined that there is no gas leak.

[0071] In this embodiment, if it is determined that no gas leak has occurred, the sample removal process described later will be executed. If it is determined that a gas leak has occurred, the system may notify the system of this fact and then execute the sample removal process, or it may cancel the execution of the remaining processes related to the supply of sample gas.

[0072] The sample discharge process is a process in which the sample gas in the space 84 of the sample container 80 is discharged due to the pressure within that space 84. When the sample discharge process is started, the second on / off valve 50 opens from the state shown in Figure 4, and the pressurized gas and sample gas discharged from space 84 flow through the flow path, as shown in Figure 6. The flow path through which the pressurized gas and sample gas flow is represented by a dashed line in Figure 6.

[0073] Furthermore, the second on / off valve 50 is closed after a predetermined time has elapsed since it was opened. The sample discharge process ends when the second on / off valve 50 is closed. Therefore, once the sample discharge process is complete, the sample supply device 12 returns to the state shown in Figure 4, and the sample gas discharged from the space 84 of the sample container 80 is captured in the sample loop 70.

[0074] Following the sample extraction process, the sample supply process is performed. The sample supply process involves supplying carrier gas from the carrier gas supply unit 54 into the sample loop 70, thereby supplying the sample gas in the sample loop 70 to the destination.

[0075] When the sample supply process begins, the hexagonal valve 72 switches from the first state, i.e., the state shown in Figure 4, to the second state. As shown in Figure 7, a portion of the sample gas trapped in the sample loop 70 is supplied to the destination along with the carrier gas supplied from the carrier gas supply unit 54. The flow paths of the carrier gas and sample gas are shown by dashed lines in Figure 7.

[0076] The hexagonal valve 72 returns to the first state after a predetermined time has elapsed since switching from the first state to the second state. The sample supply process ends when the hexagonal valve 72 returns to the first state.

[0077] Thus, according to the sample supply device 12 of this embodiment, if it is determined that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32 from the connecting channel before the pressurization process, the execution of the pressurization process can be stopped or the like can be stopped.

[0078] Furthermore, in this embodiment, the first determination process may be omitted, and instead, a notification process may be performed. However, in this case, the notification process is a process that notifies the pressure in the connecting channel based on the reference signal. Also, in this case, an operation to stop the execution of the sample gas supply process may be received by the gas chromatograph 10 or the operation reception unit 76.

[0079] 4. Specific examples of the electrical configuration of the sample supply device Figure 8 is a functional block diagram showing a specific example of the electrical configuration of the sample supply device 12 in this embodiment. Note that the RAM 104 and other components are omitted from the illustration in Figure 8.

[0080] The memory unit 106 stores threshold data 108 and reference data 110, etc. The threshold data 108 is data indicating a pressure value that is set as a threshold. For example, the threshold data 108 indicates a pre-set pressure value of the pressurized gas.

[0081] Reference data 110 is data corresponding to the reference signal. Therefore, reference data 110 indicates the detection result from the pressure sensor 44, that is, the pressure value detected by the pressure sensor 44. Although not shown in the diagram, as described above, the storage unit 106 also stores the control program and execution data.

[0082] The device control unit 100 functions as a pressure detection processing unit 112, a signal generation processing unit 114, a determination processing unit 116, a notification processing unit 118, a pressurization stop processing unit 120, a pressurization processing unit 122, a sample extraction processing unit 124, and a sample supply processing unit 126, etc., when the CPU 102 (see Figure 3) executes a control program.

[0083] The pressure detection processing unit 112 performs processing corresponding to the first pressure detection process. Before processing by the pressurization processing unit 122, the pressure detection processing unit 112 detects the pressure in the connecting channel based on the detection signal from the pressure sensor 44, with the first on / off valve 38 closed and the insertion tube 68 inserted into the space 84 inside the sample container 80.

[0084] The signal generation processing unit 114 generates a signal based on the detection result from the pressure detection processing unit 112. This signal is stored in the storage unit 106 as reference data 110.

[0085] The determination processing unit 116 performs processing corresponding to the first determination process. Based on the signal generated by the signal generation processing unit 114, the determination processing unit 116 determines whether or not there is a possibility that the sample gas will flow back into the pressurized gas supply unit 32 from the connecting channel when the pressurizing processing unit 122 opens the first on / off valve 38.

[0086] Specifically, the determination processing unit 116 determines whether or not there is a possibility of backflow of the sample gas by comparing the pressure in the connecting channel detected by the pressure detection processing unit 112 with a threshold value. In this process, the threshold data 108 and reference data 110 are referenced.

[0087] If the notification processing unit 118 determines, as a result of the determination processing unit 116, that there is a possibility that the sample gas may flow back into the pressurized gas supply unit 32 from the connection channel, it will use the notification unit 74 to notify the system of this fact.

[0088] The pressurization termination processing unit 120 terminates the processing performed by the pressurization processing unit 122 if the determination processing unit 116 determines that there is a possibility of sample gas flowing back into the pressurized gas supply unit 32 from the connecting channel.

[0089] The pressurization processing unit 122 performs processing corresponding to pressurization. With the insertion tube 68 inserted into the space 84 inside the sample container 80, the pressurization processing unit 122 opens the first on / off valve 38 and supplies pressurized gas from the pressurized gas supply unit 32 to the space 84 via the connecting channel and the insertion tube 68, thereby pressurizing the space 84.

[0090] The sample discharge processing unit 124 performs processing corresponding to the sample discharge process. After processing by the pressurizing processing unit 122, the sample discharge processing unit 124 opens the second on / off valve 50 and discharges the sample gas in the space 84 of the sample container 80 due to the pressure in that space 84.

[0091] The sample supply processing unit 126 performs processing corresponding to the sample supply process. After processing by the sample discharge processing unit 124, the sample supply processing unit 126 switches the hexagonal valve 72 from the first state to the second state, and supplies carrier gas from the carrier gas supply unit 54 into the sample loop 70, thereby supplying the sample gas in the sample loop 70 to the column 14, which is the supply destination.

[0092] The notification processing unit 118 may be configured to notify the pressure in the connection channel based on the signal generated by the signal generation processing unit 114, i.e., the reference data 110. In this case, the determination processing unit 116 and the pressurization termination processing unit 120 are omitted.

[0093] 5. Flow Figure 9 is a flowchart showing an example of the operation flow of the sample supply device 12 of this embodiment. In step S1, the hexagonal valve 72 is set to the first state, and in step S2, the first on / off valve 38 is closed. In step S3, the second on / off valve 50 is closed, and in step S4, the insertion tube 68 is inserted into the space 84 inside the sample container 76. This results in the state shown in Figure 4.

[0094] In step S5, the pressure sensor 44 detects the pressure in the connecting flow path, specifically the pressure between the first on / off valve 38 and the insertion tube 68 within that flow path.

[0095] In step S6, it is determined whether there is a possibility of the sample gas flowing back into the pressurized gas supply unit 32. Specifically, it is determined whether the pressure detected by the pressure sensor 44 is above a threshold.

[0096] If the answer in step S6 is "NO," meaning there is no possibility of the sample gas flowing back into the pressurized gas supply unit 32, proceed to step S9. On the other hand, if the answer in step S6 is "YES," meaning there is a possibility of the sample gas flowing back, proceed to step S7 and notify the system accordingly.

[0097] In step S8, the supply of sample gas to the recipient is stopped. Specifically, in step S8, the execution of the remaining processes related to the supply of sample gas is stopped.

[0098] In step S9, as shown in Figure 5, pressurized gas is supplied by opening the first on-off valve 38. After a predetermined time has elapsed since the first on-off valve 38 was opened, the first on-off valve 38 is closed in step S10. This returns the system to the state shown in Figure 4. In step S11, the pressure is detected by the pressure sensor 44, similar to step S5.

[0099] In step S12, it is determined whether a gas leak has occurred. Specifically, it is determined whether the pressure in the connecting channel has changed by more than a threshold over a predetermined period of time.

[0100] If the answer in step S12 is "NO," meaning there is no gas leak, proceed to step S13. On the other hand, if the answer in step S12 is "YES," meaning there is a gas leak, proceed to step S7 and report that fact.

[0101] In step S13, as shown in Figure 6, the second on-off valve 50 is opened to release the sample gas from the sample container 80. After a predetermined time has elapsed since the second on-off valve 50 was opened, in step S14, the second on-off valve 50 is closed to capture the sample gas in the sample loop 70. This returns the system to the state shown in Figure 4.

[0102] In step S15, as shown in Figure 7, the hexagonal valve 72 is set to the second state to supply carrier gas from the carrier gas supply unit 54 to the sample loop 70, and the sample gas captured in the sample loop 70 is supplied to the destination. In step S16, the hexagonal valve 72 is set to the first state to terminate the supply of carrier gas.

[0103] The specific configurations described in this embodiment are merely examples and can be modified as appropriate according to the actual product. For example, the configuration of the flow path in the sample supply device 12 may be modified as appropriate within the range in which the effects of the present invention can be obtained. Also, the order in which each step in the flow diagram shown in this embodiment is processed can be changed as appropriate, as long as the same result is obtained.

[0104] 6. Appearance Those skilled in the art will understand that the exemplary embodiments described above are specific examples of the following embodiments.

[0105] (Article 1) A sample supply device relating to one embodiment is: A sample supply device for supplying sample gas, which is generated in the space inside a sample container as a sample is volatilized within the container, to a destination. An insertion tube inserted into the space within the sample container, A pressurized gas supply unit is connected to the insertion tube via a flow path and supplies pressurized gas to the space via the flow path and the insertion tube to pressurize the space, A valve for opening and closing the aforementioned flow path, A pressure sensor for detecting the pressure between the valve and the insertion tube in the flow path, The system includes a control unit that receives a detection signal from the pressure sensor, The control unit, With the insertion tube inserted into the space, the pressurizing processing unit pressurizes the space by opening the valve and supplying pressurized gas from the pressurized gas supply unit to the space via the flow path and the insertion tube, After processing by the pressurizing unit, a sample extraction unit is provided to extract the sample gas from the space using the pressure within the space, Before processing by the pressurization processing unit, with the valve closed and the insertion tube inserted into the space, a pressure detection processing unit detects the pressure in the flow path based on a detection signal from the pressure sensor, The system may also include a signal generation processing unit that generates a signal based on the detection results from the pressure detection processing unit.

[0106] According to the sample supply device described in paragraph 1, with the insertion tube inserted into the space inside the sample container, the pressure in the flow path, specifically between the valve and the sample container, can be detected before supplying pressurized gas into the sample container by opening a valve provided in the flow path connecting the pressurized gas supply unit and the insertion tube.

[0107] (Paragraph 2) In the sample supply device described in Paragraph 1, The control unit may include a determination processing unit that determines, based on the signal generated by the signal generation processing unit, whether or not there is a possibility that the sample gas will flow back from the flow path to the pressurized gas supply unit when the valve is opened by the pressurization processing unit.

[0108] According to the sample supply device described in paragraph 2, it is possible to determine whether or not there is a possibility of sample gas flowing back into the pressurized gas supply section from the above-mentioned flow path before supplying pressurized gas into the sample container by opening the valve.

[0109] (3) In the sample supply device described in paragraph 2, The processing performed by the determination processing unit may include a process of comparing the pressure in the flow path detected by the pressure detection processing unit with a threshold value.

[0110] According to the sample supply device described in paragraph 3, it is possible to determine whether or not there is a possibility of backflow of the sample gas by comparing the pressure in the above-mentioned flow path with a threshold value.

[0111] (Item 4) In the sample supply device described in Item 2, The control unit may include a pressurization termination processing unit that stops the execution of processing by the pressurization processing unit when the determination processing unit determines, as a result of the determination, that there is a possibility that the sample gas may flow back from the flow path to the pressurized gas supply unit.

[0112] According to the sample supply device described in paragraph 4, if there is a possibility that the sample gas may flow back into the pressurized gas supply section from the flow path, the pressurization process is stopped, and the valve remains closed. In other words, in this case, backflow of the sample gas into the flow path is prevented, and as a result, contamination of the flow path by the sample gas is suppressed.

[0113] (Item 5) In the sample supply device described in Item 2, The control unit may include a notification processing unit that notifies the system if, as a result of the determination processing unit, it is determined that there is a possibility of the sample gas flowing back from the flow path to the pressurized gas supply unit.

[0114] According to the sample supply device described in paragraph 5, it is possible to notify the user if there is a possibility of sample gas flowing back into the above-mentioned flow path.

[0115] (Item 6) In the sample supply device described in Item 1, The control unit may include a notification processing unit that notifies the pressure in the flow path based on the signal generated by the signal generation processing unit.

[0116] According to the sample supply device described in paragraph 6, the pressure in the flow path can be notified before supplying pressurized gas into the sample container by opening the valve.

[0117] (Section 7) In the sample supply device described in Section 1, A sample loop that captures the sample gas released from the space as a result of processing by the sample release processing unit, The system further comprises a carrier gas supply unit that supplies a carrier gas for supplying the sample gas in the sample loop to a destination, The control unit, The sample supply processing unit may also include a sample supply processing unit that supplies the sample gas in the sample loop to the supply destination by supplying carrier gas from the carrier gas supply unit into the sample loop after processing by the sample extraction processing unit.

[0118] According to the sample supply device described in paragraph 7, the pressure in the flow path can be detected before supplying pressurized gas by opening the valve, and after supplying the pressurized gas, the sample gas captured by the carrier gas can be supplied to the destination.

[0119] (Clause 8) A gas chromatograph relating to one embodiment is: A sample supply device as described in any one of paragraphs 1 to 7, The device may also include a column as a destination for the sample gas supplied from the aforementioned sample supply device.

[0120] According to the gas chromatograph described in paragraph 8, the sample gas can be supplied to the column using a sample supply device that can detect the pressure in the channel for supplying the pressurized gas into the sample container before supplying the pressurized gas into the sample container. [Explanation of Symbols]

[0121] 10. Gas chromatograph 12. Sample supply device 14 columns 32 Pressurized gas supply unit 36. First gas channel 38. First on / off valve 44 Pressure Sensor 54 Carrier Gas Supply Section 66. Seventh Gas Flow Path 68 Insertion tube 70 sample loop 80 sample containers 82 samples 84 Space 100 Device Control Unit 112 Pressure detection processing unit 114 Signal Generation Processing Unit 116 Determination Processing Unit 118 Notification Processing Unit 120 Pressurization termination processing unit 122 Pressurized Processing Unit 124 Sample extraction processing unit 126 Sample supply processing unit

Claims

1. A sample supply device for supplying sample gas, which is generated in the space inside a sample container as a sample is volatilized within the container, to a destination. An insertion tube inserted into the space within the sample container, A pressurized gas supply unit is connected to the insertion tube via a flow path and supplies pressurized gas to the space via the flow path and the insertion tube to pressurize the space, A valve for opening and closing the aforementioned flow path, A pressure sensor for detecting the pressure between the valve and the insertion tube in the flow path, The system includes a control unit that receives a detection signal from the pressure sensor, The control unit, With the insertion tube inserted into the space, the pressurizing processing unit pressurizes the space by opening the valve and supplying pressurized gas from the pressurized gas supply unit to the space via the flow path and the insertion tube, After processing by the pressurizing unit, a sample extraction unit is provided to extract the sample gas from the space using the pressure within the space, Before processing by the pressurization processing unit, with the valve closed and the insertion tube inserted into the space, a pressure detection processing unit detects the pressure in the flow path based on a detection signal from the pressure sensor, A sample supply device including a signal generation processing unit that generates a signal based on the detection result in the pressure detection processing unit.

2. The sample supply apparatus according to claim 1, wherein the control unit includes a determination processing unit that determines, based on a signal generated by the signal generation processing unit, whether or not there is a possibility that the sample gas may flow back from the flow path to the pressurized gas supply unit when the valve is opened by the pressurization processing unit.

3. The sample supply device according to claim 2, wherein the processing by the determination processing unit includes a process of comparing the pressure in the flow path detected by the pressure detection processing unit with a threshold value.

4. The sample supply apparatus according to claim 2, wherein the control unit includes a pressurization termination processing unit that terminates the execution of processing by the pressurization processing unit when the determination processing unit determines, as a result of the determination, that there is a possibility that the sample gas may flow back from the flow path to the pressurized gas supply unit.

5. The sample supply apparatus according to claim 2, wherein the control unit includes a notification processing unit that notifies the user if, as a result of the determination by the determination processing unit, it is determined that there is a possibility that the sample gas may flow back from the flow path to the pressurized gas supply unit.

6. The sample supply device according to claim 1, wherein the control unit includes a notification processing unit that notifies the pressure in the flow path based on a signal generated by the signal generation processing unit.

7. A sample loop that captures the sample gas released from the space as a result of processing by the sample release processing unit, The system further comprises a carrier gas supply unit that supplies a carrier gas for supplying the sample gas in the sample loop to a destination, The control unit, The sample supply apparatus according to claim 1, further comprising a sample supply processing unit that supplies the sample gas in the sample loop to a supply destination by supplying carrier gas from the carrier gas supply unit into the sample loop after processing by the sample extraction processing unit.

8. A sample supply device according to any one of claims 1 to 7, A gas chromatograph comprising a column as a recipient for the sample gas supplied from the aforementioned sample supply device.

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