WO2018159066A1 - Régulateur de pression de gaz - Google Patents

Régulateur de pression de gaz Download PDF

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Publication number
WO2018159066A1
WO2018159066A1 PCT/JP2017/044784 JP2017044784W WO2018159066A1 WO 2018159066 A1 WO2018159066 A1 WO 2018159066A1 JP 2017044784 W JP2017044784 W JP 2017044784W WO 2018159066 A1 WO2018159066 A1 WO 2018159066A1
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WO
WIPO (PCT)
Prior art keywords
pressure
gas
liquid sample
liquid
flow path
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PCT/JP2017/044784
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English (en)
Japanese (ja)
Inventor
真悟 藤岡
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株式会社島津製作所
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Publication date
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Publication of WO2018159066A1 publication Critical patent/WO2018159066A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K17/00—Safety valves; Equalising valves, e.g. pressure relief valves
    • F16K17/02—Safety valves; Equalising valves, e.g. pressure relief valves opening on surplus pressure on one side; closing on insufficient pressure on one side
    • F16K17/04—Safety valves; Equalising valves, e.g. pressure relief valves opening on surplus pressure on one side; closing on insufficient pressure on one side spring-loaded

Definitions

  • the present invention relates to a gas pressure regulator that reduces the pressure of an inflowing gas to a predetermined pressure and causes the gas to flow out.
  • the mass spectrometer includes an ion source that ionizes components in the liquid sample, and a mass analyzer that separates and detects the ionized components according to the mass-to-charge ratio.
  • an ESI source or APCI source which is a typical ion source used to ionize a liquid sample in a mass spectrometer
  • the liquid sample is fed to an ionization probe and vaporization is promoted to the liquid sample flowing out from the tip of the ionization probe.
  • a liquid also called a nebulizer gas
  • the liquid sample When introducing the liquid sample into the ion source, for example, the liquid sample is fed into the space above the liquid surface inside the sealed liquid sample container with one end of the liquid feeding tube immersed below the liquid surface of the liquid sample. Liquid gas is supplied, and the liquid sample in the liquid sample container is supplied from the liquid supply tube to the probe of the ion source by the pressure of the liquid supply gas (for example, Patent Document 1). At this time, if the vaporization promoting gas and the liquid supply gas are supplied from a common gas source, the number of necessary gas sources can be reduced and the cost can be reduced.
  • the vaporization promoting gas and the liquid supply gas are supplied from a common gas source, the number of necessary gas sources can be reduced and the cost can be reduced.
  • FIG. 1 shows an example of a liquid sample introduction system capable of supplying a vaporization promoting gas and a liquid sending gas from a common gas source.
  • the liquid sample introduction system 100 is a system that introduces a liquid sample in a liquid sample container 170 into an ESI probe 130 disposed in an ionization chamber 110 of a mass spectrometer.
  • the liquid sample introduced into the ESI probe 130 is ionized in the ionization chamber 110, passes through the desolvation tube 111, and is subjected to analysis in a mass analysis unit provided in the subsequent stage.
  • the ESI probe 130 disposed in the ionization chamber 110 is connected to a nebulizer gas flow path 141 and a sample liquid supply flow path 160 connected to the nitrogen gas cylinder 140.
  • the ESI probe has a double-pipe structure, and a sample liquid supply channel 160 is connected to the inner tube, and a nebulizer gas channel 141 is connected to the outer tube.
  • the nebulizer gas channel 141 is provided with a valve 142 and a branch pipe 143 in order from the side closer to the nitrogen gas cylinder 140.
  • a liquid supply gas flow path 150 is connected to the branch pipe 143.
  • a gas pressure regulator (regulator) 151 and a branch pipe 152 are provided in the liquid feeding gas flow path 150, and their end portions are connected to a space above the liquid level in the liquid sample container 170.
  • a relief flow path 154 connected to the relief valve 153 is connected to the branch pipe 152.
  • the end of the sample liquid supply channel 160 is connected to the lower side (that is, in the liquid) than the liquid level in the liquid sample container 70.
  • nitrogen gas adjusted to a predetermined pressure (for example, 300 kPa) by a gas controller (not shown) from a nitrogen gas cylinder 140 is sent to the ESI probe 130 through the nebulizer gas channel 141.
  • a part of the nitrogen gas fed from the nitrogen gas cylinder 140 is also sent from the branch pipe 143 to the liquid feeding gas flow path 150.
  • the nitrogen gas supplied to the liquid supply gas flow path 150 is reduced in pressure to a predetermined pressure (for example, 100 kPa) by the regulator 151 and supplied into the liquid sample container 170.
  • a predetermined pressure for example, 100 kPa
  • the liquid sample is charged and ionized by spraying and nebulizing a nebulizer gas. At this time, if the liquid sample is not sufficiently vaporized, the ionization efficiency is deteriorated. Since the ease of vaporization varies from liquid sample to liquid sample, nebulizer gas having a pressure (for example, 150 to 500 kPa) corresponding to the type needs to be supplied to the ESI probe 130 when the liquid sample is introduced. On the other hand, it is general that a certain amount of the liquid sample itself is fed, and therefore it is necessary to feed gas to the feeding gas channel 150 at a constant pressure. As described above, the regulator 151 is used as a gas pressure regulator that feeds a gas at a constant pressure into the liquid sample container 170 while feeding nebulizer gas at different pressures depending on the liquid sample.
  • a pressure for example 150 to 500 kPa
  • FIG. 2 shows an example of a regulator 200 conventionally used. Inside the regulator 200, an inlet-side gas passage 210 and an outlet-side gas passage 230 that communicates with the inlet-side gas passage 210 via the connection part 220 are formed.
  • the inlet side gas flow path 210 side of the connection part 220 is formed in a taper shape, and an opening / closing member 240 having a shape corresponding to the taper is disposed there.
  • a partition wall 270 is provided above the outlet side gas flow path 230, and a spring 250 and a handle 260 for adjusting the length of the spring 250 are disposed above the partition wall 270.
  • a handle is previously set so that the restoring force of the spring 250 and the force of the gas in the outlet side gas flow path 230 pushing the partition wall 270 are balanced in the presence of a gas of a predetermined pressure in the outlet side gas flow path 230.
  • the spring length is adjusted by 260.
  • the present inventor has found that the secondary pressure gradually deviates from the pre-adjusted pressure. It was. As described above, the nitrogen gas after depressurization is used to send a liquid sample. Therefore, if the secondary pressure deviates, the amount of liquid sample delivered will vary, and the analysis accuracy such as the quantification of the components contained in the liquid sample will be high. There was a problem of getting worse.
  • the liquid sample introduction system used in the mass spectrometer is described as an example.
  • the pressure (primary pressure) of the gas flowing into the inlet-side gas flow path is reduced to a predetermined pressure (secondary pressure) and flows out.
  • secondary pressure a predetermined pressure
  • the problem to be solved by the present invention is to provide a gas pressure regulator capable of stabilizing the secondary pressure regardless of the fluctuation of the primary pressure.
  • the gas pressure regulator according to the present invention which has been made to solve the above problems, An inlet side gas flow path; An outlet-side gas flow path communicating with the inlet-side gas flow path via a connecting portion; An opening and closing member for opening and closing the connecting portion; An elastic member that urges the opening and closing member to close the connecting portion when the pressure inside the outlet-side gas flow path is equal to or higher than a predetermined pressure value; And a resistance tube connected to the upstream side of the inlet side gas flow path.
  • the present inventors inferred from the above measurement results as follows why the secondary pressure deviates from a predetermined pressure when the primary pressure is repeatedly changed in the conventional gas pressure regulator (regulator). .
  • a resistance tube is arranged on the upstream side of the inlet side gas flow path.
  • the gas flowing into the gas pressure regulator passes through the resistance tube and then flows into the inlet side gas flow path. For this reason, even if the primary pressure fluctuates momentarily, the fluctuation of the pressure is alleviated and a sudden change is not caused in the elastic member. Therefore, the secondary pressure can be stabilized at a predetermined pressure regardless of the fluctuation of the primary pressure.
  • the secondary pressure can be stabilized regardless of the change in the primary pressure.
  • An example of a liquid sample introduction system An example of a conventionally used regulator.
  • the principal part block diagram of one Example of the liquid sample introduction system provided with the gas pressure regulator which concerns on this invention.
  • the schematic block diagram of the gas pressure regulator of a present Example The result of having measured the change of the secondary pressure with respect to the change of the primary pressure in the liquid sample introduction system of a present Example.
  • FIG. 3 is a configuration diagram of a main part of a liquid sample introduction system 1 for a mass spectrometer provided with a gas pressure regulator 51 of the present embodiment.
  • This liquid sample introduction system 1 includes various components in an analysis liquid sample eluted from a liquid chromatograph 80 in a time-of-flight mass spectrometer (hereinafter also referred to as “TOF-MS”.
  • TOF-MS time-of-flight mass spectrometer
  • the configuration other than the ionization chamber 10 is not shown). Is used to introduce a standard liquid sample for mass calibration.
  • TOF-MS is used as an ion analyzer, but a liquid sample introduction system having a similar configuration can be used in other mass analyzers and ion analyzers (ion mobility analyzers, etc.). Can do.
  • control unit 90 Each part of the liquid chromatograph 80, the liquid sample introduction system 1, and the TOF-MS is controlled by the control unit 90.
  • the control unit 90 includes an analysis condition setting unit 92 and an analysis execution unit 93 as functional blocks.
  • the entity of the control unit 90 is a computer in which necessary software is installed, and an input unit 94 and a display unit 95 are connected to each other.
  • the analysis condition setting unit 92 sets analysis conditions based on an input by the user, creates an analysis execution file, and stores the analysis execution file in the storage unit 91.
  • the analysis execution unit 93 operates each part of the liquid chromatograph 80, the liquid sample introduction system 1, and the TOF-MS based on the analysis execution file in accordance with an instruction from the user to analyze various components in the analysis liquid sample. Execute.
  • Various components in the analysis liquid sample temporally separated by the column of the liquid chromatograph 80 are sprayed into the ionization chamber 10 as fine droplets charged by the ESI probe 20.
  • a standard liquid sample for mass calibration sent from the liquid sample introduction system 1 described later is sprayed into the ionization chamber 10 as fine droplets charged by the ESI probe 30.
  • These charged droplets collide with gas molecules in the ionization chamber 10 and are pulverized into finer droplets, which are quickly dried (desolvated) and ionized.
  • These ions are drawn into the desolvation tube 11 by the differential pressure between the ionization chamber 10 and the first intermediate vacuum chamber (the first vacuum chamber of the analysis chamber having a multistage differential exhaust system configuration) located in the subsequent stage. While being converged by the guide, it is introduced into the time-of-flight mass spectrometer in the analysis room and used for analysis.
  • the liquid sample introduction system 1 is used in the TOF-MS ionization chamber 10 together with the liquid sample eluted from the column of the liquid chromatograph 80 (or the liquid sample eluted from the column of the liquid chromatograph 80).
  • this is a system for introducing and ionizing a standard liquid sample for mass calibration.
  • Five types of standard liquid samples A to E are prepared, each of which contains components that generate a plurality of ions having different mass-to-charge ratios. Housed in containers 70a-70e.
  • the ESI probe 30 disposed in the ionization chamber 10 is provided with a nebulizer gas passage 41 connected to a nitrogen gas cylinder (atomization gas source) 40.
  • the nebulizer gas flow path 41 is provided with a valve 42 and a branch pipe 43 in order from the side closer to the nitrogen gas cylinder 40, and the liquid feed gas flow path 50 is connected to the branch pipe 43.
  • a gas pressure regulator 51 and a branch pipe 52 are provided in the liquid feeding gas flow path 50, and a relief flow path 54 connected to a relief valve 53 is connected to the branch pipe 52.
  • the gas pressure regulator 51 includes a regulator 511 having the structure shown in FIG. 4 and a resistance tube 512 provided in the inlet-side gas flow path of the regulator.
  • the resistance tube 512 is a polytetrafluoroethylene (PTFE) (Teflon (registered trademark)) tube having a length of 1 m and an inner diameter of 0.5 mm.
  • PTFE polytetrafluoro
  • the liquid feed gas flow path 50 is branched into five liquid feed gas sub-flow paths 50 a to 50 e on the downstream side of the branch pipe 52.
  • the ends of the liquid feeding gas sub-channels 50a to 50e are connected to the space above the liquid level in the containers (liquid sample containers) 70a to 70e in which standard liquid samples are stored.
  • an air release flow path 56 connected to the air release valve 55 is provided in parallel with each of the liquid feed gas sub flow paths 50a to 50e.
  • the ESI probe 30 is connected to the sample liquid feeding channel 60.
  • the other end of the sample feeding channel 60 is connected to the main port 61g of the 6-position 7-way valve 61.
  • the 6-position 7-way valve 61 has six sub-ports 61a to 61f, and one of the sub-ports 61a to 61f is connected to the main port 61g.
  • One end of each of the sample liquid feeding sub flow paths 60a to 60e is connected to each of the sub ports 61a to 61e.
  • the other ends of the sample liquid feeding sub-channels 60a to 60e are connected below the liquid level in the liquid sample containers 70a to 70e (that is, in the liquid).
  • one end of an air release channel 62 is connected to the sub port 61f.
  • the other end of the air release channel 62 is open to the atmosphere.
  • the liquid sample introduction operation using the liquid sample introduction system 1 of the present embodiment will be described. Since the liquid samples contained in the liquid sample containers 70a to 70e have different vaporization characteristics (ease of vaporization), the optimum nebulizer gas pressure is different. For example, the liquid sample A accommodated in the liquid sample container 70a is most easily vaporized and can be vaporized by spraying a nebulizer gas having a pressure of 150 kPa. On the other hand, the liquid sample B is most difficult to vaporize and needs to be vaporized by spraying a nebulizer gas having a pressure of 550 kPa.
  • the analysis execution unit 93 controls the gas controller to operate the valve 42 and supplies the nebulizer gas having the optimum pressure for the selected liquid sample to the nebulizer gas channel 41. That is, in the liquid sample introduction system 1 of the present embodiment, nebulizer gas is supplied in a pressure range of 150 kPa to 550 kPa according to the type of liquid sample to be introduced. In addition, these pressure notations mean the pressure with respect to the pressure in the ionization chamber 10.
  • the nebulizer gas is supplied at a pressure of 601.325 kPa.
  • the liquid supply amount of each liquid sample is constant, and the liquid supply gas is supplied to the liquid sample containers 70a to 70e in which the liquid samples are stored at a constant pressure (100 kPa in this embodiment). Therefore, the gas pressure regulator 51 maintains a constant secondary pressure (100 kPa) regardless of the pressure (primary pressure, 150 kPa to 550 kPa) in the nebulizer gas channel 41 that varies depending on the liquid sample introduced into the ESI probe 30. It is necessary to reduce the pressure. In the state where the supply of the nebulizer gas is stopped, the pressure in the nebulizer gas channel 41 is 0 kPa, and when the liquid sample B is used from this state, the primary pressure varies by 550 kPa.
  • the elastic member 250 typically a spring
  • the expansion and contraction length varies.
  • the relationship between the preset pressure (secondary pressure) and the spring length has shifted, and the secondary pressure has gradually shifted from the pressure adjusted in advance.
  • the liquid sample feeding speed varies due to the fluctuation of the secondary pressure, particularly when the liquid sample is slowed down
  • the liquid sample sent last time remains in the sample feeding channel 160, and the mass peak of the liquid sample becomes the mass peak of the actual sample. May overlap.
  • the output voltage of the detector during auto-tuning for optimizing the analysis conditions differs, which makes it difficult to compare the sensitivity between samples.
  • the resistance tube 512 is disposed in the inlet-side gas flow path of the regulator 511. Therefore, even if a sudden pressure fluctuation occurs, the fluctuation is alleviated, and the spring length Does not change rapidly. Therefore, the above-mentioned problem does not occur and the secondary pressure can be stabilized.
  • the present inventor performed two measures against changes in primary pressure (changes in flow rate in measurement) when the above-described gas pressure regulator 51 was used in the liquid sample introduction system 1 of the above embodiment.
  • the change in the secondary pressure was confirmed and compared with the conventional one using only the regulator. The results will be described below.
  • the set value of the secondary pressure was 100 kPa.
  • a regulator product name: AR20 (K) manufactured by SMC Corporation is used as the regulator, and similarly to the above, as the resistance tube 512, polytetrafluoroethylene (PTFE: 1 m in length and 0.5 mm in inner diameter) is used. polytetrafluoroethylene) tube was used. In the comparative example, only the regulator was used. The nebulizer gas flow rate was 3 L / min, and the measurement was performed at room temperature of 20 ° C. The resistance value (conductance) of the resistance tube 512 at the time of measurement in this example is obtained as follows.
  • P is the pressure of the nebulizer gas (primary pressure, 550 kPa)
  • r is the radius of the resistance tube (2.5 ⁇ 10 -4 m)
  • L is the length of the resistance tube (1 m)
  • ⁇ is nitrogen gas at 20 ° C
  • the viscosity (0.0175 mPa ⁇ s).
  • Fig. 5 shows changes in secondary pressure when the flow rate of nebulizer gas is changed in the order of 1L / min, 2L / min, 3L / min, 2L / min, 1L / min, 3L / min, 1L / min. .
  • the difference between the initial value of the secondary pressure (101.979 kPa) and the maximum fluctuation value of the pressure during measurement (the pressure value with the largest difference between the initial value and 83.326 kPa) was 18.653 kPa.
  • the difference between the initial value of the secondary pressure (99.439 kPa) and the maximum fluctuation value of the pressure during measurement (102.113 kPa) is 2.674 kPa. It has decreased to. From the measurement result of the secondary pressure, it can be seen that the secondary pressure is stable by arranging the resistance tube 512 in the inlet-side gas flow path of the regulator 511 as in the present embodiment.
  • FIG. 5 shows changes in the secondary pressure when the nebulizer gas flow rate is changed, including the operation of starting the nebulizer gas delivery from the stop of the nebulizer gas delivery.
  • the flow rate of the nebulizer gas is 2 L / min (10 s), Open to atmosphere (20 s), 2 L / min (60 s), 3 L / min (30 s), Open to atmosphere (20 s), L 3 L / min (60 s) Changed in order.
  • the difference between the initial value of the secondary pressure (100.251 kPa) and the maximum fluctuation value of the pressure during measurement (89.842 kPa) was 10.409 kPa.
  • the difference between the initial value (98.347 kPa) of the secondary pressure and the maximum fluctuation value (105.427 kPa) of the pressure during measurement is reduced to 7.08 kPa. From the measurement result of the secondary pressure, it can be seen that the secondary pressure is stable by arranging the resistance tube in the inlet side gas flow path of the regulator as in this embodiment.
  • the above embodiment is merely an example, and can be changed as appropriate in accordance with the gist of the present invention.
  • the example in which the gas pressure regulator is used in the liquid sample introduction system that introduces the liquid sample into the mass spectrometer has been described.
  • the present invention is not limited to this, and the configuration is such that the fluctuating primary pressure is reduced to a predetermined secondary pressure.
  • the gas pressure regulator of the present invention can be used in various apparatuses that require the above.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
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Abstract

La présente invention concerne un régulateur de pression de gaz 51 caractérisé en ce qu'il est pourvu d'un canal d'écoulement de gaz côté entrée 210, un canal d'écoulement de gaz côté sortie communiquant avec le canal d'écoulement de gaz côté entrée 210 par l'intermédiaire d'une partie de raccordement 220, un élément d'ouverture/fermeture 240 pour ouvrir et fermer la partie de raccordement 220, un élément élastique 250 pour pousser l'élément d'ouverture/fermeture 240 de façon à fermer la partie de raccordement 220 lorsque la pression à l'intérieur du canal d'écoulement de gaz côté sortie 230 est égale ou supérieure à une pression prédéfinie, et un tube de résistance 512 raccordé à un côté amont du canal d'écoulement de gaz côté entrée 210.
PCT/JP2017/044784 2017-03-02 2017-12-13 Régulateur de pression de gaz WO2018159066A1 (fr)

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JP2017-000916U 2017-03-02
JP2017000916U JP3210394U (ja) 2017-03-02 2017-03-02 ガス圧調整器

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WO2018159066A1 true WO2018159066A1 (fr) 2018-09-07

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU192665U1 (ru) * 2019-05-20 2019-09-25 Хисамов Флюс Фанилович Регулятор расхода
RU193443U1 (ru) * 2019-05-31 2019-10-29 Хисамов Флюс Фанилович Регулятор расхода

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7188441B2 (ja) * 2018-04-05 2022-12-13 株式会社島津製作所 質量分析装置および質量分析方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0232043U (fr) * 1988-08-25 1990-02-28
JPH10170412A (ja) * 1996-12-06 1998-06-26 Ohbayashi Corp ガス捕集器具
JP2001249722A (ja) * 2000-03-03 2001-09-14 Kanbishi:Kk 圧力調整器

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0232043U (fr) * 1988-08-25 1990-02-28
JPH10170412A (ja) * 1996-12-06 1998-06-26 Ohbayashi Corp ガス捕集器具
JP2001249722A (ja) * 2000-03-03 2001-09-14 Kanbishi:Kk 圧力調整器

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU192665U1 (ru) * 2019-05-20 2019-09-25 Хисамов Флюс Фанилович Регулятор расхода
RU193443U1 (ru) * 2019-05-31 2019-10-29 Хисамов Флюс Фанилович Регулятор расхода

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