WO2017017765A1 - Dispositif de raccordement automatique de tube - Google Patents

Dispositif de raccordement automatique de tube Download PDF

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Publication number
WO2017017765A1
WO2017017765A1 PCT/JP2015/071262 JP2015071262W WO2017017765A1 WO 2017017765 A1 WO2017017765 A1 WO 2017017765A1 JP 2015071262 W JP2015071262 W JP 2015071262W WO 2017017765 A1 WO2017017765 A1 WO 2017017765A1
Authority
WO
WIPO (PCT)
Prior art keywords
needle
pressure
fluid
pipe
column
Prior art date
Application number
PCT/JP2015/071262
Other languages
English (en)
Japanese (ja)
Inventor
努 大古場
Original Assignee
株式会社島津製作所
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 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to PCT/JP2015/071262 priority Critical patent/WO2017017765A1/fr
Priority to JP2017530502A priority patent/JP6516010B2/ja
Publication of WO2017017765A1 publication Critical patent/WO2017017765A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/08—Preparation using an enricher
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns

Definitions

  • the present invention provides an automatic pipe that automatically connects pipes to a container member such as an analysis column, a trap column, and an extraction container through which a fluid is passed in a liquid chromatograph or a supercritical fluid chromatograph using a needle seal structure.
  • the present invention relates to a connection device.
  • a needle seal structure as a structure for connecting pipes easily and quickly.
  • the needle provided at the tip of the pipe is inserted into the opening provided in the object to be connected, so that the inner peripheral surface of the opening and the outer peripheral surface of the needle tip are in line contact and the pipe is to be connected.
  • the needle seal structure is used for an injection port in an autosampler of a liquid chromatograph, for example.
  • Patent Document 1 proposes that the extraction container can be easily attached to and detached from the apparatus by connecting the pipe to the extraction container of the supercritical fluid component extraction apparatus using the above needle seal structure.
  • a plurality of extraction containers are installed in the apparatus, and movable needles are connected to these extraction containers by a needle seal structure, so that piping connection to the extraction containers to be used is automatically performed by moving the needles. It is also proposed to change it.
  • the needle seal structure is used, not only the piping connection to the extraction container in the supercritical fluid component extraction apparatus but also the piping connection to the analysis column or trap column in the liquid chromatograph can be automatically performed.
  • the residual pressure does not release immediately even after the mobile phase liquid supply is stopped, and immediately after the mobile phase liquid supply is stopped, the pipe connection needle is connected to a column, etc.
  • the container member is separated from the container member, there is a problem that the liquid is ejected from the needle tip or the opening of the container member. This is particularly noticeable when a mobile phase having a high compression rate is used.
  • a fixed time is set as a “depressurization time” for decreasing the residual pressure after the mobile phase liquid supply is stopped, and the needle is moved after the fixed time has elapsed. It is conceivable to take a method of pulling out from the container member. However, since the actual residual pressure varies depending on the flow rate of the liquid and the type of mobile phase, if the pressure release time is set short, the needle is not sufficiently reduced until the residual pressure is sufficiently reduced due to insufficient pressure release time. Will be pulled out and liquid will be ejected. Therefore, it is necessary to set the pressure release time longer than necessary.
  • an object of the present invention is to optimize the timing for detaching the pipe from the container member in an automatic pipe connecting device that attaches / detaches the pipe to / from the container member by the needle seal structure.
  • One embodiment of an automatic pipe connecting device includes a fluid feeding pipe for feeding a fluid, a needle provided at one end of the fluid feeding pipe, and a fluid feeding by inserting the needle.
  • a needle seal structure that allows fluid communication between the pipe and the internal space is provided at one end, and a needle for connecting or disconnecting the needle to the container member and a container member that allows fluid to flow in the internal space.
  • a needle drive mechanism for moving the pressure sensor, a pressure sensor for detecting the pressure in the fluid feed pipe, and a pressure state determination unit for judging whether or not the fluid feed pipe is in a pressurized state based on a detection value of the pressure sensor;
  • a control unit configured to control the operation of the needle drive mechanism, and based on the determination result of the pressure state determination unit, the needle is not detached from the container member when the fluid feeding pipe is in a pressurized state; It includes those were.
  • the inside of the fluid delivery pipe is in a pressurized state means that the pressure in the fluid delivery pipe is higher than the atmospheric pressure.
  • a pressure sensor for detecting the pressure in the fluid feed pipe, and whether or not the fluid feed pipe is in a pressurized state based on the detection value of the pressure sensor.
  • the pressure state judging unit that performs the control and the controller configured to prevent the needle from being detached from the container member when the inside of the fluid feeding pipe is in a pressurized state are provided.
  • the needle is not detached from the container member, and the liquid can be prevented from being ejected from the needle tip or the opening of the container member.
  • the needle can be detached from the container member at an appropriate timing without waiting for the needle for an unnecessarily long time after stopping the delivery of the mobile phase. It becomes possible to shorten the time required for analysis.
  • the control unit is configured to connect the needle to one container member selected from the plurality of container members. Is preferred. Then, the container member to be used can be automatically changed by moving the needle.
  • a sample is once captured in a trap column and concentrated, and then the concentrated sample is guided to an analysis column for separation analysis.
  • An autosampler 4 for injecting a sample is provided on the mobile phase liquid flow path 6 for concentration.
  • the concentration mobile phase feeding flow path 6 is a path through which the concentration mobile phase is fed by the liquid feed pump 2.
  • the concentration mobile phase liquid flow path 6 is connected to one of the ports provided in the rotary high pressure valve 8.
  • the high pressure valve 8 is a two-position valve having six ports and switching the connection between adjacent ports.
  • Each port of the high-pressure valve 8 includes a concentration mobile phase liquid flow path 6, a drain, a column inlet flow path 10, a column outlet flow path 14, an analysis mobile phase liquid flow path 18 and an analysis flow path 20. It is connected.
  • the high-pressure valve 8 is provided between the concentration mobile phase liquid flow path 6 and the column inlet flow path 10, between the column outlet flow path 14 and the drain, and to the analysis mobile phase liquid flow path 18 and the analysis flow path 20.
  • concentration mode The state shown in FIG. 6; hereinafter referred to as the concentration mode
  • analysis mode One of a state in which the channel 18 is connected and the column outlet channel 14 and the analysis channel 20 are connected.
  • the column inlet channel 10 is connected to the inlet 39 (see FIG. 2) of the column connecting device 12 (automatic pipe connecting device), and the column outlet channel 14 is connected to the outlet 52 (see FIG. 2) of the column connecting device 12.
  • the column connection device 12 will be described later, a trap column for concentrating the sample is accommodated in the column connection device 12.
  • the mobile phase feeding flow path for analysis 18 is a flow path through which the mobile phase fed by the mobile phase feeding apparatus 16 flows.
  • the mobile phase liquid feeding device 16 includes liquid feeding pumps 16a and 16b for feeding different solvents, and a mixer 16c for mixing the solvents fed by the liquid feeding pumps 16a and 16b.
  • an analysis column 22 for separating a sample for each component, and a detector 24 for detecting the sample component separated by the analysis column 22.
  • the column connection device 12 will be described with reference to FIG.
  • the inlet 39 and the outlet 52 are provided in the casing of the column connection device 12.
  • the column inlet channel 10 is connected to the inlet 39, and the column outlet channel 14 is connected to the outlet 52.
  • the inlet 39 is connected to the upper needle 38 via a pipe 40 (fluid feed pipe).
  • the upper needle 38 is moved by the needle drive mechanism 44 in the horizontal plane direction and the vertical direction with the tip thereof directed vertically downward.
  • a plurality of lower needles 28 are provided at a position below the upper needle 38.
  • the lower needle 28 is supported by a support table 30 with the tip thereof facing vertically upward.
  • Each lower needle 28 is connected to a port of a rotary column selection valve 46 through a flow path 45.
  • the column selection valve 46 has a common port at the center, and an outlet channel 50 leading to the outlet 52 is connected to the common port.
  • the column selection valve 46 selectively switches and connects any one of the lower needles 28 to the outlet channel 50 by rotating the rotor provided with the channel 48.
  • a trap column 32 (container member) is installed above each lower needle 28.
  • the trap column 32 is installed on the lower needle 28 while being held by the rack 31.
  • Needle seal structures 34 and 36 are provided at the lower end and the upper end of each trap column 32, respectively.
  • the needle seal structure is an opening that communicates with the internal space. By inserting the needle tip into the opening, the needle seal structure is in line contact with the outer peripheral surface of the needle tip so that the inner space and the inner flow path of the needle are kept liquid-tight. It is a structure that allows communication.
  • the tip of the lower needle 28 is inserted and connected to the needle seal structure 34 at the lower end of each trap column 32.
  • the needle seal structure 36 at the upper end of each trap column 32 is for inserting and connecting the upper needle 38.
  • a pressure sensor 42 is provided on the proximal end side of the upper needle 38.
  • the pressure sensor 42 detects the pressure in the pipe 40.
  • the pressure value detected by the pressure sensor 42 is taken into the control device 56 via the control unit 54 described later (see FIG. 3).
  • the concentration feeding pump 2, the analysis feeding device 16, the autosampler 4, the high pressure valve 8 and the column exchange device 12 are connected to a common control device 56.
  • the control device 56 is realized by, for example, a general-purpose personal computer or a dedicated computer.
  • the column connection device 12 is provided with a control unit 54 that controls the operation of the needle drive mechanism 44 and the column selection valve 46.
  • the control unit 54 is a computer dedicated to the column connection device 12.
  • the detection signal of the pressure sensor 42 is taken into the control device 56 via the control unit 54.
  • the control device 56 includes an analysis operation management unit 58, a pressure state determination unit 60, and a threshold value holding unit 62.
  • the analysis operation management unit 58 manages the operations of the concentration liquid delivery pump 2, the analysis liquid delivery device 16, the autosampler 4, the high-pressure valve 8, and the column exchange device 12 so that a series of analysis operations to be described later is executed. Is.
  • the pressure state determination unit 60 applies the pressure in the pipe 40 when the upper needle 38 is connected to one of the trap columns 32 by comparing the output signal of the pressure sensor 42 with a preset threshold value. It is comprised so that it may determine whether it is a pressure state.
  • the threshold value used by the pressure state determination unit 60 is set based on, for example, the atmospheric pressure measured in advance. The set threshold value is held in the threshold value holding unit 62. When the output signal of the pressure sensor 42 exceeds the threshold value, the pressure state determination unit 60 determines that the inside of the pipe 40 is in a pressurized state.
  • the upper needle 38 is connected to the trap column 32 to be used, the high-pressure valve 8 is set to the concentration mode, and the feeding of the concentration mobile phase is started (see FIG. 6). Then, the sample is injected into the concentration mobile phase liquid flow path 6 by the autosampler 4, and the sample is captured by the trap column 32.
  • the high pressure valve 8 is set to the sample introduction mode, the analysis mobile phase is fed by the analysis mobile phase feeding device 16, and the sample is introduced into the analysis channel 20 (FIG. 7). reference.).
  • the sample captured by the trap column 32 is guided to the analysis column 22 and separated for each component. Sample components separated by the analysis column 22 are detected by a detector 24.
  • the mobile phase liquid feeding by the analysis mobile phase liquid feeding device 16 is stopped. Immediately after stopping the mobile phase liquid feeding, the trap column 32, the upper needle 38, and the inside of the pipe 40 are pressurized by the residual pressure. If the upper needle 38 is detached from the trap column 32 in this state, there is a problem that liquid is ejected from the tip of the upper needle 38 or the opening of the needle seal structure 36 at the upper end of the trap column 32 and the inside of the apparatus is contaminated. is there.
  • the pressure in the pipe 40 is monitored by the pressure sensor 42 so that the upper needle 38 is not detached from the trap column 32 when the inside of the pipe 40 is in a pressurized state. Whether or not the pressure in the pipe 40 is in a pressurized state is determined by comparing the output value of the pressure sensor 42 with a preset threshold value.
  • FIG. 5 is a graph showing an example of the time change of the pressure in the pipe 40 detected by the pressure sensor 40. As shown in this graph, there is a residual pressure in the pipe 40 immediately after the mobile phase liquid feeding is stopped, and the residual pressure decreases with time. Then, when the output value of the pressure sensor 40 becomes equal to or less than a threshold value (for example, atmospheric pressure + 10%) set based on the atmospheric pressure, the upper needle 38 is separated from the trap column 32, whereby the inside of the pipe 40 is It drops to atmospheric pressure. Thereby, the ejection of the liquid from the tip of the needle 38 or the trap column 32 can be prevented.
  • a threshold value for example, atmospheric pressure + 10%
  • the automatic pipe connection device is applied to a concentrated liquid chromatograph.
  • the automatic pipe connection device of the present invention includes a plurality of extraction containers in a supercritical fluid extraction apparatus, and the extraction container to be used is needle-sealed. It can also be applied as a device that automatically changes depending on the pipe connection by structure. Further, the present invention can also be applied as a device that includes a plurality of analysis columns used for separating a sample of a liquid chromatograph and that changes the analysis column used by pipe connection with a needle seal structure.

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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)
  • Pathology (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

La présente invention concerne un dispositif de raccordement automatique de tube pourvu d'un capteur de pression destiné à détecter la pression à l'intérieur d'un tube d'alimentation en fluide, d'une unité de détermination d'état de pression destinée à déterminer si l'intérieur du tube d'alimentation en fluide est sous pression sur la base d'une valeur de détection provenant du capteur de pression, et d'une unité de commande conçue de façon à empêcher qu'une aiguille ne se sépare d'un élément récipient lorsque l'intérieur du tube d'alimentation en fluide est sous pression.
PCT/JP2015/071262 2015-07-27 2015-07-27 Dispositif de raccordement automatique de tube WO2017017765A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2015/071262 WO2017017765A1 (fr) 2015-07-27 2015-07-27 Dispositif de raccordement automatique de tube
JP2017530502A JP6516010B2 (ja) 2015-07-27 2015-07-27 自動配管接続装置

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2015/071262 WO2017017765A1 (fr) 2015-07-27 2015-07-27 Dispositif de raccordement automatique de tube

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WO2017017765A1 true WO2017017765A1 (fr) 2017-02-02

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PCT/JP2015/071262 WO2017017765A1 (fr) 2015-07-27 2015-07-27 Dispositif de raccordement automatique de tube

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WO (1) WO2017017765A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018173214A1 (fr) * 2017-03-23 2018-09-27 株式会社日立ハイテクノロジーズ Support de boîtier de colonne de séparation, dispositif de remplacement de colonne de séparation et procédé de remplacement
WO2018189966A1 (fr) * 2017-04-11 2018-10-18 株式会社島津製作所 Dispositif d'extraction de constituants
WO2019006710A1 (fr) * 2017-07-05 2019-01-10 深圳迈瑞生物医疗电子股份有限公司 Dispositif d'analyse en phase liquide et procédé d'analyse de dispositif d'analyse en phase liquide
WO2021171508A1 (fr) * 2020-02-27 2021-09-02 株式会社島津製作所 Dispositif de réception de colonne et chromatographe en phase liquide
JP7058402B1 (ja) 2021-02-26 2022-04-22 株式会社プレッパーズ 液体クロマトグラフ用ノズル及び液体クロマトグラフ
JP2022132242A (ja) * 2021-02-26 2022-09-07 株式会社プレッパーズ カラムユニット

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Publication number Priority date Publication date Assignee Title
JP2005278438A (ja) * 2004-03-29 2005-10-13 Fuji Photo Film Co Ltd 自動核酸分離精製方法およびその装置
JP2014160055A (ja) * 2013-01-22 2014-09-04 Shimadzu Corp 超臨界流体成分抽出装置

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5880269B2 (ja) * 2012-05-15 2016-03-08 株式会社島津製作所 分取精製装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005278438A (ja) * 2004-03-29 2005-10-13 Fuji Photo Film Co Ltd 自動核酸分離精製方法およびその装置
JP2014160055A (ja) * 2013-01-22 2014-09-04 Shimadzu Corp 超臨界流体成分抽出装置

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2018173214A1 (ja) * 2017-03-23 2019-11-07 株式会社日立ハイテクノロジーズ 分離カラム収納ホルダ、分離カラム交換装置及び交換方法
WO2018173214A1 (fr) * 2017-03-23 2018-09-27 株式会社日立ハイテクノロジーズ Support de boîtier de colonne de séparation, dispositif de remplacement de colonne de séparation et procédé de remplacement
WO2018189966A1 (fr) * 2017-04-11 2018-10-18 株式会社島津製作所 Dispositif d'extraction de constituants
JPWO2018189966A1 (ja) * 2017-04-11 2020-02-20 株式会社島津製作所 成分抽出装置
US20200147515A1 (en) * 2017-04-11 2020-05-14 Shimadzu Corporation Component extraction apparatus
US11565193B2 (en) 2017-04-11 2023-01-31 Shimadzu Corporation Component extraction apparatus
US11204338B2 (en) 2017-07-05 2021-12-21 Shenzhen Mindray Bio-Medical Electronics Co., Ltd. Liquid phase analysis device and analysis method for liquid phase analysis device
WO2019006710A1 (fr) * 2017-07-05 2019-01-10 深圳迈瑞生物医疗电子股份有限公司 Dispositif d'analyse en phase liquide et procédé d'analyse de dispositif d'analyse en phase liquide
WO2021171508A1 (fr) * 2020-02-27 2021-09-02 株式会社島津製作所 Dispositif de réception de colonne et chromatographe en phase liquide
JPWO2021171508A1 (fr) * 2020-02-27 2021-09-02
JP7347645B2 (ja) 2020-02-27 2023-09-20 株式会社島津製作所 カラム収容装置及び液体クロマトグラフ
JP7058402B1 (ja) 2021-02-26 2022-04-22 株式会社プレッパーズ 液体クロマトグラフ用ノズル及び液体クロマトグラフ
JP2022131302A (ja) * 2021-02-26 2022-09-07 株式会社プレッパーズ 液体クロマトグラフ用ノズル及び液体クロマトグラフ
JP2022132242A (ja) * 2021-02-26 2022-09-07 株式会社プレッパーズ カラムユニット
JP7336104B2 (ja) 2021-02-26 2023-08-31 株式会社プレッパーズ カラムユニット

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JPWO2017017765A1 (ja) 2017-12-28
JP6516010B2 (ja) 2019-05-22

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