WO2023157135A1 - ガスクロマトグラフ質量分析装置 - Google Patents

ガスクロマトグラフ質量分析装置 Download PDF

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Publication number
WO2023157135A1
WO2023157135A1 PCT/JP2022/006208 JP2022006208W WO2023157135A1 WO 2023157135 A1 WO2023157135 A1 WO 2023157135A1 JP 2022006208 W JP2022006208 W JP 2022006208W WO 2023157135 A1 WO2023157135 A1 WO 2023157135A1
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WO
WIPO (PCT)
Prior art keywords
gas
gas chromatograph
mass spectrometer
vacuum
supply
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2022/006208
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English (en)
French (fr)
Japanese (ja)
Inventor
良朗 平松
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
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Shimadzu Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP2024500777A priority Critical patent/JP7593525B2/ja
Priority to PCT/JP2022/006208 priority patent/WO2023157135A1/ja
Publication of WO2023157135A1 publication Critical patent/WO2023157135A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components

Definitions

  • the present invention relates to a gas chromatograph mass spectrometer, and more particularly to a gas chromatograph mass spectrometer that has an explosion prevention function when hydrogen carrier gas is used.
  • FIG. 1 shows an example of a gas chromatograph mass spectrometer, which is composed of a gas chromatograph section GC on the left side and a mass spectrometry section MS on the right side.
  • a sample is put into the sample injection section 1 and the vaporized sample is introduced into the column 2 by the carrier gas CG supplied to the injection section 1 .
  • Column 2 is optionally heated by column oven 3 .
  • the tip of column 2 is introduced into the MS section.
  • a sample (gas) emitted from the column 2 is ionized by the ion source 4, converged and accelerated by the ion lens 5, separated by the mass-to-charge ratio (m/z) of the sample by the quadrupole filter 6 or the like, and sent to the detector 7. detected by
  • a roughing pump RVP also called a low vacuum pump or foreline pump
  • a high vacuum pump such as a turbomolecular pump TMP capable of reducing pressure to about 10 -7 Pa or a diffusion pump is used in combination.
  • FIG. 2 is a flow chart showing an example of the operating procedure of the gas chromatograph-mass spectrometer.
  • step S1 the supply of carrier gas to the GC section is started.
  • step S2 the roughing pump RVP of the MS section is operated.
  • step 3 the vacuum gauge S1 for measuring the degree of vacuum in the analysis chamber 8 in FIG. 1 is set to proceed to the next step S4 when the degree of vacuum (DoV) reaches a predetermined value, for example, 300 Pa or less. be done.
  • DoV degree of vacuum
  • step S4 the turbo molecular pump TMP is driven in order to further increase the degree of vacuum.
  • step S5 the operational status of the turbo-molecular pump is determined to be a "TMP Ready" state when, for example, the number of revolutions of the pump reaches a predetermined number of revolutions or more within a certain period of time. Start temperature control.
  • step S3 the process proceeds to step S7 and the roughing pump RVP is stopped. Further, if the rotational speed of the turbo-molecular pump does not reach the "TMP Ready" state in step S5, driving of the turbo-molecular pump TMP and roughing pump RVP is stopped in step S8.
  • a vacuum pump such as a roughing pump in the MS section was started. This is because if the carrier gas is allowed to flow after the degree of vacuum in the MS section is increased, the sample in the column may also spread into the MS section and contaminate the analysis chamber.
  • the carrier gas When hydrogen gas is used as the carrier gas, there is a risk of explosion if the carrier gas fills the analysis chamber or the main body case of the device containing the analysis chamber, for example, if the concentration of hydrogen reaches 4 to 75%. . Therefore, as shown in FIG. 2, when the vacuum pump is stopped in step S7 or step S8, the leak valve LV of the analysis chamber is operated in step S9, or the door arranged on the side of the analysis chamber is forcibly closed. It is configured to open and release hydrogen gas to the outside of the MS section.
  • each pump is automatically stopped if there is an abnormality in the vacuum pump, but the supply of carrier gas is not stopped.
  • mass spectrometers in which leak valves and door opening mechanisms do not operate normally, and in which these safety devices themselves are not provided in the first place.
  • there is also an error in the operation procedure such as not starting the vacuum pump even though the carrier gas has started flowing, and the danger of hydrogen gas explosion in the mass spectrometer is still high.
  • the present invention has been made to solve the above problems, and its object is to provide a gas chromatograph mass spectrometer that prevents the explosion of hydrogen gas in advance and improves safety. be.
  • the mass spectrometer which has been made to solve the above problems, is as follows.
  • a supply operation means for starting or stopping the supply of a carrier gas used in the gas chromatograph part, and a vacuum inside the analysis tube of the mass spectrometry part and evaluation means for evaluating the vacuum state in the analysis tube, and when the evaluation means determines that the vacuum state is normal after starting to drive the vacuum pump, the supply operation means is a gas chromatograph mass spectrometer equipped with a gas control means for controlling and starting the supply of carrier gas.
  • the start of carrier gas supply in the caschromatograph section is always controlled according to the vacuum state inside the analysis tube of the mass spectrometry section.
  • the degree of vacuum does not reach a predetermined value due to failure of the vacuum pump or the like, the supply of the carrier gas is not started, making it possible to prevent explosion of the hydrogen gas.
  • FIG. 4 Schematic diagram of a gas chromatograph mass spectrometer.
  • 4 is a flow chart showing an example of an operation procedure of a gas chromatograph mass spectrometer
  • 1 is a block diagram showing a control circuit of a gas chromatograph mass spectrometer according to the present invention
  • FIG. 4 is a flow chart showing an example of the operating procedure of the gas chromatograph-mass spectrometer according to the present invention.
  • FIG. A feature of the gas chromatograph-mass spectrometer of the present invention is that the start of supply of the carrier gas used in the gas chromatograph section is controlled according to the vacuum state in the analysis tube of the mass spectrometer section.
  • FIG. 3 is a block diagram showing an example of an electric circuit used in the gas chromatograph-mass spectrometer.
  • FIG. 3 clearly shows a supply operation means GV for starting and stopping the supply of the carrier gas CAG used in the gas chromatograph section (GC).
  • the supply operation means is a gas valve provided in the middle of a pipe connecting a cylinder (not shown) filled with a carrier gas and the sample injection part 1, and the valve is opened and closed according to a signal from the control circuit. It has a control mechanism to control.
  • a pressure gauge S2 for measuring the inflow pressure of the carrier gas into the column is shown on the way from the supply part of the carrier gas CG to the column 2.
  • This pressure gauge S2 is not indispensable in the present invention, but it is an important part for improving the analysis accuracy of the sample in the gas chromatograph section. It is also a useful part for checking whether the gas valve control and the pressure control of the gas flow controller separately provided in the carrier gas supply line are properly performed.
  • a vacuum gauge S1, a roughing pump RVP, and a turbomolecular pump TMP are clearly shown in the mass spectrometry unit MS in FIG.
  • the gas chromatograph section GC and the mass spectrometry section MS include various devices and parts other than those shown in FIG. 3. FIG. there is
  • C1 in FIG. 3 is a control circuit that controls the gas chromatograph section GC
  • C2 is a control circuit that controls the mass spectrometry section MS.
  • a control circuit may be provided for each device, or a control circuit C in which the control circuits C1 and C2 are integrated into one.
  • An input means IN such as a numeric keypad or a touch panel and a display means DIS such as a monitor are connected to each of the control circuits C1 and C2.
  • the input means IN and the display means DIS may be provided for each device.
  • the control line L1 is a signal line for controlling the supply operation means GV according to instructions from the control circuit C1.
  • the control line L2 is a signal line for inputting the detected value from the pressure gauge S2 to the control circuit C1.
  • Other equipment/parts of the gas chromatograph section are connected to the control circuit C1 via the control line L3.
  • the control line L4 is a signal line for inputting the detected value of the vacuum gauge to the control circuit C2.
  • the control line L5 serves as a signal line for controlling the driving of the turbomolecular pump TMP and a signal line for outputting the driving state of the TMP (eg, whether the pump is running or not, the number of rotations).
  • the control line L6 serves as a signal line for controlling the driving of the roughing pump RVP and a signal line for outputting the driving state of the RVP.
  • the control line L7 is a signal line that connects other devices/parts of the mass spectrometry unit MS and the control circuit C2.
  • the control circuit C1 and the control circuit C2 are connected to each other by the control line L0, and perform processing of each control circuit based on the mutual control state.
  • the gas chromatograph mass spectrometer of the present invention controls the start and stop of supply of carrier gas for safety measures.
  • a control unit (control function) for controlling such a carrier gas supply operation means may be provided in either the control circuit C1 or C2. It is preferably provided in the controlling control circuit.
  • the input means IN or the display means DIS and the control circuit C1 or C2 are connected by respective control lines L8 to L11.
  • FIG. 4 is a flow chart showing the operating procedure of the gas chromatograph-mass spectrometer of the present invention.
  • step S100 the roughing pump RVP is driven, and in step S101, it is evaluated whether the degree of vacuum DoV in the analysis tube has reached a predetermined value, for example, 300 Pa or less. If it does not reach the predetermined value, the roughing pump RVP is stopped, and in step 107, the leak valve LV and the door are opened. These may be performed at the same time, but the leak valve LV may be opened first, and the door may be opened when the leak valve is broken or otherwise malfunctions.
  • a predetermined value for example, 300 Pa or less.
  • the "evaluation means for evaluating the vacuum state” means whether or not the detected value of the vacuum gauge for measuring the degree of vacuum in the analysis tube has reached a predetermined standard. , means to determine whether or not the rotation speed of the vacuum pump has reached a predetermined reference, as will be described later. If necessary, it is also possible to add to the determination condition whether or not the vacuum pump is in a driving state.
  • step S101 When the degree of vacuum DoV has reached a predetermined value in step S101, the supply operation means GV is operated to start supplying the carrier gas in step S102. At the same time, the turbo-molecular pump TMP is started to be driven. If the supply of the carrier gas and the driving of the turbomolecular pump are not performed at the same time, the supply of the carrier gas is started and then the turbomolecular pump is operated in order to prevent the sample from contaminating the inside of the analysis tube.
  • step S103 it is confirmed from the detected value of the pressure gauge S2 that the pressure control of the carrier gas (control of the gas valve and flow controller) is within the set value range (referred to as "Gas Ready” state). Also, it is confirmed that the rotation speed of the turbo molecular pump TMP reaches a predetermined rotation speed or more within a predetermined time (“TMP Ready” state). When these conditions are satisfied, temperature adjustment of the ion source of the MS section is started in step S104.
  • step S106 the supply of carrier gas (CG) is stopped, and the turbo molecular pump TMP and roughing pump RVP are stopped. Then, in step S107, the above leak valve and door are opened.
  • CG carrier gas
  • the vacuum state in the analysis tube is evaluated by "TMP Ready” in step S101 or step S103, and the start (S102) or stop (S106) of carrier gas supply is controlled (gas control means).
  • the gas control means (control mechanism) is provided in the control circuit C1 of the gas chromatograph section in FIG. , the carrier gas supply operating means GV can also be controlled. If the communication means between the control means C1 and C2 does not operate due to some problem such as disconnection of the control line L0, the control means C1 controls to stop the supply of the carrier gas. Safety can be improved.
  • (Section 1) In a gas chromatograph mass spectrometer that combines a gas chromatograph part and a mass spectrometry part, supply operation means for starting or stopping the supply of the carrier gas used in the gas chromatograph; a vacuum pump for evacuating the analysis tube of the mass spectrometer; and evaluation means for evaluating the vacuum state in the analysis tube,
  • the gas chromatograph mass spectrometer is provided with gas control means for controlling the supply operation means and starting supply of the carrier gas when the evaluation means determines that the vacuum state is normal after starting to drive the vacuum pump.
  • (Section 2) In the gas chromatograph mass spectrometer according to the above item 1, A communication means for connecting the gas chromatograph unit and the mass spectrometry unit, The gas control means is a gas chromatograph mass spectrometer that controls the supply operation means to stop the supply of the carrier gas when it is detected that the communication means is not operating.
  • the gas chromatograph unit comprises selection means for selecting the type of carrier gas, A gas chromatograph mass spectrometer in which the gas control means operates only when the selection means selects a specific gas.
  • the gas control means of the present invention can be operated. It becomes possible to drive the gas control means of the invention.
  • the evaluation means is a gas chromatograph mass spectrometer that evaluates the vacuum state based on the detected value of a vacuum gauge that measures the degree of vacuum in the analysis tube or the driving state of the vacuum pump.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
PCT/JP2022/006208 2022-02-16 2022-02-16 ガスクロマトグラフ質量分析装置 Ceased WO2023157135A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2024500777A JP7593525B2 (ja) 2022-02-16 2022-02-16 ガスクロマトグラフ質量分析装置
PCT/JP2022/006208 WO2023157135A1 (ja) 2022-02-16 2022-02-16 ガスクロマトグラフ質量分析装置

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Application Number Priority Date Filing Date Title
PCT/JP2022/006208 WO2023157135A1 (ja) 2022-02-16 2022-02-16 ガスクロマトグラフ質量分析装置

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61112265U (https=) * 1984-12-27 1986-07-16
JPS63243864A (ja) * 1987-03-31 1988-10-11 Shimadzu Corp ガスクロマトグラフ質量分析計インタ−フエイス
US20210199631A1 (en) * 2018-06-01 2021-07-01 Micromass Uk Limited A gc/ms arrangement and mass spectrometer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61112265U (https=) * 1984-12-27 1986-07-16
JPS63243864A (ja) * 1987-03-31 1988-10-11 Shimadzu Corp ガスクロマトグラフ質量分析計インタ−フエイス
US20210199631A1 (en) * 2018-06-01 2021-07-01 Micromass Uk Limited A gc/ms arrangement and mass spectrometer

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JPWO2023157135A1 (https=) 2023-08-24

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