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JP-7855935-B2 - Sample supply device and gas chromatograph

JP7855935B2JP 7855935 B2JP7855935 B2JP 7855935B2JP-7855935-B2

Inventors

  • 山本 善丈
  • 青野 晃

Assignees

  • 株式会社島津製作所

Dates

Publication Date
20260511
Application Date
20220615

Claims (8)

  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 the signal generated by the signal generation processing unit, whether or not there is a possibility of sample gas flowing 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 apparatus 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 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.
  5. The sample supply apparatus according to claim 2, wherein the control unit includes a notification processing unit that notifies the system if, as a result of the determination by the determination processing unit, it is determined that there is a possibility of sample gas flowing back from the flow path to the pressurized gas supply unit.
  6. The sample supply apparatus 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.

Description

This invention relates to a sample supply device and a gas chromatograph for supplying sample gases. For example, in a sample introduction device such as the one disclosed in Patent Document 1 below, a sample in a sample container with a space called a headspace formed at the top is heated, causing a gas containing volatile components of the sample (sample gas) to be stored in the headspace. When collecting the sample gas into the sample loop, a needle (insertion tube) is inserted into the sample container, and pressurized gas is supplied to the headspace within the sample container via this needle. This pressurizes the headspace, allowing the sample gas to be drawn into the sample loop by the pressure within the headspace. International Publication No. 2014/038019 This is a schematic diagram showing an example of the configuration of the gas chromatograph in this embodiment.This is a schematic diagram showing an example of the configuration of the sample supply device of this embodiment.This is a block diagram showing an example of the electrical configuration of the sample supply device of this embodiment.This is a diagram illustrating the operation of the sample supply device of this embodiment.This is a diagram illustrating the operation of the sample supply device of this embodiment.This is a diagram illustrating the operation of the sample supply device of this embodiment.This is a diagram illustrating the operation of the sample supply device of this embodiment.This is a functional block diagram showing a specific example of the electrical configuration of the sample supply device of this embodiment.This is a flowchart showing an example of the operation flow of the sample supply device of this embodiment. 1. Configuration of the Gas Chromatograph Figure 1 is a schematic diagram showing an example of the configuration of the gas chromatograph 10 of this embodiment. The gas chromatograph 10 includes a sample supply device 12, a column 14, a detector 16, and the like. 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. Column 14 is heated in a column oven 18. Each component in the sample gas introduced into column 14 is separated as it passes through the column and detected by detector 16. 2. Configuration of the Sample Supply Device Figure 2 is a schematic diagram showing an example of the configuration of the sample supply device 12 of this embodiment. Specifically, the sample supply device 12 of this embodiment is a device for supplying sample gas generated in the space 84 inside the sample container 80 when the sample 82 is volatilized inside the sample container 80 to a destination. The space 84 is a so-called headspace and is formed above the sample 82 inside the sample container 80. The 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, an airflow 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, and a six-way valve 72, among other components. The pressure control unit 30 is connected to a carrier gas supply source (not shown in the diagram), such as a gas cylinder. It adjusts the carrier gas pressure to a constant pressure greater than atmospheric pressure and then supplies it as pressurized gas. The pressure of the pressurized gas can be preset. The pressure control unit 30 includes a pressurized gas supply unit 32 and a pressurized gas discharge unit 34. The pressurized gas supply unit 32 is connected to a first gas passage 36, and the pressurized gas discharge unit 34 is connected to a third gas passage 48. Pressurized gas at a constant pressure is supplied to the first gas passage 36 from the pressurized gas supply unit 32. The pressurized gas in the third gas passage 48 is discharged from the pressurized gas discharge unit 34. 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. A first on/off valve 38 is provided in the first gas flow path 36. The first on/off valve 38 is a general-purpose, electrically controllable valve such as a solenoid valve. 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