WO2009118825A1 - Chromatographe à gaz - Google Patents

Chromatographe à gaz Download PDF

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Publication number
WO2009118825A1
WO2009118825A1 PCT/JP2008/055542 JP2008055542W WO2009118825A1 WO 2009118825 A1 WO2009118825 A1 WO 2009118825A1 JP 2008055542 W JP2008055542 W JP 2008055542W WO 2009118825 A1 WO2009118825 A1 WO 2009118825A1
Authority
WO
WIPO (PCT)
Prior art keywords
insert
injector
sample
region
base
Prior art date
Application number
PCT/JP2008/055542
Other languages
English (en)
Japanese (ja)
Inventor
尚弘 西本
正樹 叶井
正憲 西野
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/JP2008/055542 priority Critical patent/WO2009118825A1/fr
Priority to JP2010505066A priority patent/JP4840532B2/ja
Publication of WO2009118825A1 publication Critical patent/WO2009118825A1/fr

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Classifications

    • 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
    • G01N30/16—Injection
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02—Burettes; Pipettes
    • B01L3/0241—Drop counters; Drop formers
    • B01L3/0268—Drop counters; Drop formers using pulse dispensing or spraying, eg. inkjet type, piezo actuated ejection of droplets from capillaries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00378—Piezoelectric or ink jet dispensers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/02—Adapting objects or devices to another
    • B01L2200/026—Fluid interfacing between devices or objects, e.g. connectors, inlet details
    • B01L2200/027—Fluid interfacing between devices or objects, e.g. connectors, inlet details for microfluidic devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0832—Geometry, shape and general structure cylindrical, tube shaped
    • B01L2300/0838—Capillaries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0433—Moving fluids with specific forces or mechanical means specific forces vibrational forces
    • B01L2400/0439—Moving fluids with specific forces or mechanical means specific forces vibrational forces ultrasonic vibrations, vibrating piezo elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0442—Moving fluids with specific forces or mechanical means specific forces thermal energy, e.g. vaporisation, bubble jet
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography

Definitions

  • the present invention relates to a gas chromatograph, and more particularly to a gas chromatograph provided with an injector for discharging a sample by a piezoelectric element.
  • a gas chromatograph has a configuration in which an inlet of a separation column is connected to an insert, a liquid sample is injected into the insert using a microsyringe, vaporized, and the vaporized sample is placed on a carrier gas and sent into the separation column.
  • Injectors and inserts need to be replaced due to dirt, etc., and precise alignment between the injector and the insert is required every time it is replaced, so there are problems such as complicated and time-consuming operations for injector replacement and insert replacement. there were. Therefore, there is a demand for easy replacement of injectors and inserts while ensuring positioning accuracy.
  • An object of the present invention is to provide a gas chromatograph provided with a mechanism that can realize the alignment accuracy at the time of injector replacement with a simple structure and can thermally separate the injector from the insert.
  • the gas chromatograph apparatus is configured such that the injector and the insert are connected by a member having a positioning function to perform alignment.
  • the member having the positioning mechanism includes a heating mechanism for heating the insert and a heat insulating portion between the injector and the insert, so that the insert is heated in a state in which heat is not easily transmitted to the injector portion, and the sample is It has a structure that can be vaporized.
  • the gas chromatograph according to the present invention includes an injector that discharges a sample by a piezoelectric element, a sample inlet that receives a sample discharged from the injector, a heating unit that heats and vaporizes the received sample, and an exhaust that discharges the vaporized sample.
  • An insert having an outlet, a base for positioning the injector and the insert, a heater arranged to heat the insert in the insert heating region of the base, a sample outlet of the injector, and a sample inlet of the insert are shared.
  • a sealed container having a carrier gas supply port to which carrier gas is supplied so as to be included in the internal space, a separation column connected to the discharge port of the insert, and a detector connected downstream of the separation column ing.
  • the base In order to position the injector and the insert relative to each other, the base is inserted so that the injector area having the first positioning portion for positioning the injector, the center of the discharge port of the injector and the center of the sample inlet of the insert are on the same straight line And an insert region having a second positioning portion for positioning.
  • the base is provided with a heat insulating region arranged between the injector region and the insert region in order to thermally separate the injector region and the insert region.
  • the insert has a cylindrical outer shape.
  • the base is made of a silicon substrate
  • the second positioning portion is a groove having a V-shaped cross section formed by anisotropic wet etching of the silicon substrate. The insert is positioned by being fitted into the groove of the second positioning portion.
  • a separation column is a capillary column.
  • the insert is connected to the capillary column so that its internal space communicates with the capillary column, and the sample inlet of the insert has a diameter of 1 mm or less.
  • the insert volume needs to correspond to the volume increase at the time of sample vaporization, but since it is for a small amount sample of about nL as a liquid, it is about ⁇ L in a gas state, has a diameter of 1 mm or less, and several mm There is no problem with the length of insert.
  • the injector one having a rectangular flat bottom surface can be used.
  • the first positioning portion is a recess having a flat surface formed on the base, and the bottom surface of the recess is formed in a shape that matches the shape of the bottom surface of the injector, the injector is in the recess. Positioning is performed by fitting.
  • the heat insulating region can be a region made of porous silicon dioxide formed on the base.
  • the heat insulating region made of porous silicon dioxide is specifically described later, but by selectively treating the silicon substrate between the injector region and the insert region, the silicon substrate is integrated with the injector region and the insert region. Can be formed.
  • a preferable example of the heater is a metal thin film resistor formed on a base.
  • the distance between the injector and the insert can be made constant, and the center of the injector outlet and the center of the sample inlet of the insert can be aligned.
  • the gas chromatograph of the present invention it is possible to easily perform positioning at the time of injector replacement while corresponding to the introduction of a small amount of sample using an ink jet type injector, so that the replacement time of the injector can be greatly shortened, Performance degradation due to poor alignment is prevented and stable measurement is possible.
  • FIG. 1A is for showing the outline of the sample injection part of the gas chromatograph of one Example.
  • FIG. 1B is a front view of the same embodiment.
  • FIG. 1C is a cross-sectional view taken along the line CC of FIG. 1A.
  • FIG. 1D is a cross-sectional view showing a connection state between the insert and the capillary column.
  • FIG. 2 is a perspective view showing the base and the injector and the insert positioned and fixed to the base.
  • FIG. 3 is a process diagram illustrating a method of manufacturing a base in the order of processes.
  • FIG. 1A to 1D are schematic configuration diagrams of a gas chromatograph of one embodiment.
  • FIG. 1A is a plan view of a sample injection portion, and shows a part in a sectional view through a sealed container.
  • FIG. 1B is a front view of the same embodiment, showing the sealed container and the insert through.
  • 1C is a cross-sectional view taken along the line CC in FIG. 1A
  • FIG. 1D is a cross-sectional view showing a connection state between the insert and the capillary column.
  • FIG. 2 is a perspective view showing the base and the injector and the insert positioned and fixed to the base.
  • the base 2 is made of a silicon substrate, and the injector 4 and the insert 6 are positioned and fixed.
  • the injector 4 is of an ink jet type in which a sample is ejected by a piezoelectric element, and has an outer shape of a rectangular parallelepiped and a rectangular flat bottom surface.
  • a sample supply pipe that has a discharge port 8 for discharging a sample at the tip surface of the injector 4, that is, the end surface facing the insert 6 when positioned on the base 2, and a sample is supplied from the outside to the opposite end surface 10 is connected.
  • An actuator 12 made of a piezoelectric element is provided on the upper surface of the injector 4 in order to discharge the sample supplied from the sample supply pipe 10 as a droplet from the discharge port 8.
  • the base 2 has an injector region 13 for positioning the injector 4 on the base 2, and a concave portion 14 having a flat bottom surface is formed in the injector region 13 as a first positioning portion for positioning the injector 4. .
  • the bottom surface of the concave portion 14 is formed in a shape that matches the bottom surface shape of the injector 2, and the injector 2 is positioned by being fitted into the concave portion 14.
  • a pressing spring 16 is provided in order to fix the injector 4 in the recess 14 of the base 2.
  • the holding spring 16 has a base end fixed to the hermetic container 18, and the injector 4 is fixed in a state of being positioned with respect to the base 2 by pressing the injector 4 toward the base 2 at the tip end.
  • the insert 6 has a cylindrical outer shape, and has a sample inlet 20 that receives a sample discharged from the injector 4, a heating unit 22 that heats and vaporizes the received sample, and an outlet 24 that discharges the vaporized sample.
  • An end of the capillary column 26 is inserted into the discharge port 24 as a separation column.
  • the inner space of the insert 6 communicates with the capillary column 26, and the central axis of the insert 6 and the central axis of the capillary column 26 are the same.
  • the insert 6 and the capillary column 26 are connected so as to be in a straight line.
  • the insert 6 has an outer diameter of 500 ⁇ m, and the sample inlet 20 has a diameter of, for example, 300 ⁇ m.
  • an insert region 28 is provided in the base 2.
  • a groove 28 having a V-shaped cross section is formed as a second positioning portion so that the center of the discharge port 8 of the injector 4 and the center of the sample inlet 20 of the insert are on the same straight line.
  • the groove 28 is formed by anisotropic wet etching of the silicon substrate of the base 2 with an alkaline solution.
  • the insert 6 is positioned by being fitted into the groove 28.
  • the insert 6 is also fixed by being pressed by an appropriate member (not shown) such as a holding spring.
  • a heater 32 is provided in the insert region 28 of the base 2 so as to heat the heating part 22 of the insert 6.
  • the heater 32 is made of a Ni—Cr alloy or the like, and is a metal thin film resistor having a thickness of 1 to 10 ⁇ m formed by vapor deposition or sputtering through a mask having an opening in a predetermined region of the insert region 28. Lead wires 34 and 36 for energization are connected to the heater 32.
  • a heat insulating region 38 made of porous silicon dioxide is formed between the injector region 13 and the insert region 28.
  • the heat insulating region 38 is for preventing the heat of the heater 32 from being transmitted to the injector region 13.
  • the heat insulating region 38 is formed so as to reach from the surface to the bottom surface in the thickness direction of the base 2 over the entire width of the base 2 in order to thermally shield between the injector region 13 and the insert region 28.
  • a sealed container 18 covering the injector 4 and the insert 6 is provided.
  • a carrier gas supply port 40 through which gas is supplied is provided.
  • the sample supply pipe 10 penetrates the sealed container 18 and is connected to the injector 4 from the outside, the capillary column 26 penetrates the sealed container 18 and is guided to the outside, and the lead wires 34 and 36 also penetrate the sealed container 18 to the outside. Has been led to.
  • the sealed container 18 covers the sample discharge port 8 of the injector 4 and the sample inlet 20 of the insert 6 in a common internal space, and the carrier gas is supplied from the carrier gas supply port 40 to the internal space, whereby the insert 6
  • the sample that has been injected into and vaporized is fed into the capillary column 26 by the carrier gas and separated.
  • a detector 42 is connected downstream of the capillary column 26.
  • an FID hydrogen flame ionization detector
  • the discharge amount of the ink jet injector 4 of this embodiment is smaller than that of a conventional microsyringe, and is usually about several pL to several tens of nL / 1 drop.
  • the injector 4 is manufactured in a chip shape using MEMS (micro electro mechanical system) technology, and its outer shape is usually determined by cutting using a precision processing machine such as a dicing saw. Therefore, it is produced with an accuracy of the order of ⁇ m.
  • MEMS micro electro mechanical system
  • the tolerance is about ⁇ 20 ⁇ m.
  • the silicon substrate 50 to be the base 2 has a surface crystal plane of (100) and has a low resistivity.
  • the silicon substrate 50 is thermally oxidized to form an oxide film 52 on the surface.
  • This oxide film 52 becomes a protective film for later etching.
  • a silicon nitride film may be formed by a technique such as CVD (chemical vapor deposition).
  • a photomask pattern is transferred to the photoresist layer 54 on the oxide film 52 by photolithography, and an opening 56 for forming a recess for positioning the injector and a V-groove for positioning the insert are formed.
  • an opening 58 is formed.
  • the opening 58 for forming the V-groove is rectangular, and its longitudinal direction is aligned with the ⁇ 110> axial direction of the silicon substrate 50.
  • the oxide film 52 in the openings 56 and 58 is removed by wet etching using a chemical solution such as buffered hydrofluoric acid or by dry etching using a gas such as CF 4 .
  • the photoresist layer 54 is removed, and etching is performed using a chemical solution capable of anisotropic etching with different etching rates depending on the silicon crystal orientation, such as KOH (potassium hydroxide) and TMAH (tetramethylammonium hydroxide).
  • KOH potassium hydroxide
  • TMAH tetramethylammonium hydroxide
  • the recess opening 56 for positioning the injector has a large etching area, the etching of the (100) plane is finished before the line intersecting the (111) plane appears, and the recess 14 having a flat bottom surface is formed. It is formed.
  • the following process is a process for forming a thermal insulating layer made of porous silicon oxide (see Non-Patent Document 2).
  • an Au thin film 60 is formed by vapor deposition on the surface of the silicon substrate 50 where the recesses 14 and the grooves 30 are formed.
  • a resist pattern is formed on the surface of the Au thin film 60 by photolithography, and etching is performed with an Au etchant to selectively remove the Au thin film in the region where the thermal insulating layer is to be formed or to form the opening 62.
  • the opening 62 is formed so as to cross the surface of the silicon substrate 50 in the width direction.
  • the portion is converted into a porous silicon layer 64.
  • the porous silicon layer 64 formed by anodization is formed isotropically and has a depth of about 300 ⁇ m.
  • a heater 22 is formed by forming a metal film serving as a resistor by a mask vapor deposition method or a mask sputtering method.
  • the silicon substrate 50 having a thickness of about 300 ⁇ m it can be made porous in the entire thickness direction in the step (7).
  • the recess 14 at the fixed position of the injector chip is formed with a depth of about 200 ⁇ m. If an injector chip having a discharge port height of about 500 ⁇ m from the bottom surface of the chip is used, the straight line connecting the injector discharge port and the sample inlet of the insert is 200 ⁇ m above the silicon substrate surface. On the other hand, if the depth of the V-groove 30 is 205 ⁇ m from the surface of the silicon substrate, when an insert having an outer diameter of 500 ⁇ m is used, it is in line with the discharge port of the injector.
  • the injector chip 4 and the insert 6 are arranged on the base 2 of the alignment member manufactured as described above. Since the bottom surface of the recess 14 for arranging the injector chip 4 is formed according to the shape of the bottom surface of the injector chip, it can be fixed at a position aligned with the center of the insert 6.
  • the fixing is exemplified by fixing with the presser spring 16 in consideration of chip replacement, but is not limited to this as long as the chip can be easily replaced.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

L’invention a pour objet la précision de positionnement lors du remplacement d’un injecteur par un arrangement simple et par séparation thermique de l’injecteur d’un insert. Selon l’invention, une carte de base (2) comprend une zone d’injecteur (13) muni d’une première pièce de positionnement (14) pour le positionnement d’un injecteur (4) afin d’obtenir le positionnement mutuel de l’injecteur (4) et d’un insert (6), et une zone d’insert (28) munie d’une deuxième pièce de positionnement (30) pour le positionnement de l’insert (6) de sorte que le centre d’un port de décharge (8) de l’injecteur (4) et le centre d’une entrée d’échantillon (20) de l’insert (6) se trouvent sur la même ligne droite. La carte de base (2) comprend en outre une zone d’isolation thermique (38) disposée entre la zone d’injecteur (13) et la zone d’insert (28) afin de les séparer thermiquement.
PCT/JP2008/055542 2008-03-25 2008-03-25 Chromatographe à gaz WO2009118825A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2008/055542 WO2009118825A1 (fr) 2008-03-25 2008-03-25 Chromatographe à gaz
JP2010505066A JP4840532B2 (ja) 2008-03-25 2008-03-25 ガスクロマトグラフ

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2008/055542 WO2009118825A1 (fr) 2008-03-25 2008-03-25 Chromatographe à gaz

Publications (1)

Publication Number Publication Date
WO2009118825A1 true WO2009118825A1 (fr) 2009-10-01

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WO (1) WO2009118825A1 (fr)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002207027A (ja) * 2001-01-11 2002-07-26 Shimadzu Corp 微小流路を有する樹脂製部材の作製方法、その方法により作製された部材およびそれを用いた計測装置
WO2008026241A1 (fr) * 2006-08-28 2008-03-06 Shimadzu Corporation Chromatographe en phase gazeuse

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000137034A (ja) * 1998-10-30 2000-05-16 Shimadzu Corp 液体注入装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002207027A (ja) * 2001-01-11 2002-07-26 Shimadzu Corp 微小流路を有する樹脂製部材の作製方法、その方法により作製された部材およびそれを用いた計測装置
WO2008026241A1 (fr) * 2006-08-28 2008-03-06 Shimadzu Corporation Chromatographe en phase gazeuse

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
FUMIHIRO ENDO ET AL.: "Inkjet Chip o Mochiita Shiryo Donyu ni yoru Gas Chromatography", SEPARATION SCIENCE 2005 KOEN YOSHISHU, 28 July 2005 (2005-07-28), pages 103 - 104 *
P.STEINER ET AL.: "Micromachining applications of porous silicon", THIN SOLID FILMS, vol. 255, no. 1/2, 15 January 1995 (1995-01-15), pages 52 - 58, XP004010502, DOI: doi:10.1016/0040-6090(95)91137-B *
TAKAHIDE NISHIYAMA ET AL.: "Inkjet Microchip o Mochiiru Gas Chromatography no Tame no Cho Biryo Injector no Kaihatsu", JOURNAL OF JAPAN SOCIETY FOR ANALYTICAL CHEMISTRY, vol. 54, no. 6, 5 June 2005 (2005-06-05), pages 533 - 539 *
TATSURO NAKAGAMA: "Gas Chromatograph-yo Cho Biryo Biryo Injector", BUNSEKI, no. 8, 5 August 2007 (2007-08-05), pages 385 - 388 *

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JP4840532B2 (ja) 2011-12-21
JPWO2009118825A1 (ja) 2011-07-21

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