WO2017104747A1 - Colonne - Google Patents

Colonne Download PDF

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Publication number
WO2017104747A1
WO2017104747A1 PCT/JP2016/087375 JP2016087375W WO2017104747A1 WO 2017104747 A1 WO2017104747 A1 WO 2017104747A1 JP 2016087375 W JP2016087375 W JP 2016087375W WO 2017104747 A1 WO2017104747 A1 WO 2017104747A1
Authority
WO
WIPO (PCT)
Prior art keywords
column
tube
outer tube
less
inner tube
Prior art date
Application number
PCT/JP2016/087375
Other languages
English (en)
Japanese (ja)
Inventor
雅道 高橋
黒田　充
Original Assignee
株式会社 潤工社
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
Priority claimed from JP2016111569A external-priority patent/JP2017215304A/ja
Application filed by 株式会社 潤工社 filed Critical 株式会社 潤工社
Publication of WO2017104747A1 publication Critical patent/WO2017104747A1/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
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/56—Packing methods or coating methods
    • 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
    • G01N30/60—Construction of the column

Definitions

  • the present invention relates to a column used for high-efficiency liquid chromatography (hereinafter referred to as HPLC).
  • HPLC high-efficiency liquid chromatography
  • This conventional column includes a metal only (for example, SUS), a resin only (for example, polyetheretherketone, hereinafter referred to as PEEK), a metal outer tube, and a resin inner.
  • a metal only for example, SUS
  • a resin only for example, polyetheretherketone, hereinafter referred to as PEEK
  • PEEK polyetheretherketone
  • What consists of tubes is known.
  • a column composed of only metal when analyzing a substance having a high metal coordination property, adsorption occurs on the inner surface of the column, and the analysis accuracy may deteriorate.
  • a column composed only of a resin has a problem that pressure resistance is poor, and there is a possibility that quality stability is impaired.
  • a column composed of a metal outer tube and a resin inner tube cannot be reduced in diameter.
  • the filler is finely and uniformly filled, and as shown in FIG. 5 (b), the filler is non-uniformly filled. This is because the gaps between the particles vary and affect the passage speed of the sample passing through the column, and the analysis accuracy is lowered. In this way, when the packing material is packed in the column, the packing material is not sufficiently packed in the column because the flow rate of the packing material is different between the inside and the outside of the column. There is a possibility that a tailing phenomenon that pulls the tail occurs and the accuracy of the analysis result is significantly lowered.
  • the abrasion resistance test is performed by polishing a column inner tube with a grinder (air grinder) with a predetermined roughness (# 1000) under a predetermined pressure (at least 0.25 N). Refers to a test. Even in the column after this test, the number of theoretical plates per unit length is about 400.
  • the filler is not affected by the unevenness of the inner surface and can be filled smoothly, and the filler can be packed more finely and uniformly, Analysis accuracy can be further improved.
  • the column inner tube is composed of polyetheretherketone.
  • FIG. 1 It is a figure which shows the structure of the column of this invention. It is sectional drawing of a column main body.
  • A is a figure which shows typically the relationship between the filler in a comparative example, and a column inner tube
  • (b) is a figure which shows typically the relationship between the filler in an embodiment, and a column inner tube. It is a figure which shows the difference in the analysis result of HPLC
  • (a) is a figure which shows the result of a comparative example
  • (b) is a figure which shows the result of embodiment.
  • FIG. It is a figure which shows typically the passage speed of the sample by the number of theoretical plates of a filler, (a) is a figure with which the filler is packed finely and uniformly, and (b) is filled with the filler non-uniformly.
  • FIG. It is a figure which shows the packing state of the filler by the surface roughness of the pipe
  • a column 1 according to this embodiment includes a column main body 2, nuts 3 and 3 provided at both ends of the column main body 2, and a packing material (silica gel with a particle diameter of 2 ⁇ m) ( (Not shown).
  • a packing material silicon gel with a particle diameter of 2 ⁇ m
  • the column outer tube 4 and the nuts 3 and 3 manufactured by cutting are prepared.
  • the column outer tube 4 has a through hole having an inner diameter of 1 to 5 mm (2 mm in this embodiment).
  • a PEEK tube constituting the column inner tube 5 is manufactured by extrusion molding.
  • the tube manufactured here has an outer diameter of 1.9 mm and a wall thickness of 0.45 mm.
  • the tube is inserted into the through hole of the column outer tube 4, and after sealing one end of the column outer tube 4, nitrogen gas is injected into the tube from the other end side at a temperature of 155 ° C.
  • Comparative Example 1 is different from the above embodiment in that the column inner tube is formed by cutting, and the other configurations are the same.
  • the column manufacturing method according to Comparative Example 1 prepares the column outer tube 4 and the nuts 3 and 3 as in the column according to the embodiment.
  • a cylindrical resin rod (made by PEEK) having an outer diameter of 2 mm is prepared.
  • the resin rod is inserted into the through hole of the column outer tube 4.
  • a through hole having an inner diameter of 1 mm is formed by cutting along the central axis in the longitudinal direction of the inserted resin rod.
  • Comparative Example 2 will be described.
  • a tube to be the column inner tube 5 is prepared with a predetermined sample length (50 mm), and a core material (manufactured by SUS) 10 is inserted into the tube.
  • a digital force gauge AD-4932A, manufactured by A & D.
  • a grindstone with a predetermined roughness # 1000 (outside diameter 4 mm) is attached to an air grinder (TRUSCO, TMAG10SN) which becomes a polishing machine (only the following grindstone with a shaft is shown) 12, and the rotational speed Rotate at 60000 rpm.
  • the value of 4 times is only in one axial direction, and the “step” is a plane, so 4 in each of the two axial directions (the horizontal axis in the previous figure and the longitudinal axis with respect to the page).
  • a difference of 16 times that of the present invention occurs.
  • the depth of the recess is not 4 times in all the pipes in the column, and there are some offsets, it is 4 minutes rather than simply reducing the theoretical plate number to 1/16. It was settled in about 1 of.
  • the number of theoretical plates is generally expressed by the following equation. N: number of theoretical plates tr : holding time W: peak width
  • the packing material can be packed finely and uniformly, and the analysis accuracy is improved.

Abstract

La présente invention aborde le problème consistant à fournir une colonne pour chromatographie en phase liquide à haute performance (HPLC) dans laquelle la précision d'analyse et la stabilité de qualité d'un dispositif d'analyse sont améliorées. À cet effet, la colonne selon la présente invention est caractérisée en ce qu'elle comprend un tube externe de colonne cylindrique formé de métal et un tube interne de colonne positionné sur la surface interne du tube externe de colonne intimement fixé à la forme de la surface interne, le volume du tube interne de colonne étant de 9 à 4200 mm3, et le tube interne de colonne étant tel que, après qu'une charge d'au moins 0,25 N est appliquée dans un test de résistance au frottement, la rugosité moyenne arithmétique (Ra) de la surface interne est de 0,1 µm ou moins et la hauteur maximale (Ry) est de 1,5 μm ou moins.
PCT/JP2016/087375 2015-12-16 2016-12-15 Colonne WO2017104747A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
JP2015245726 2015-12-16
JP2015-245726 2015-12-16
JP2016084785 2016-04-20
JP2016-084785 2016-04-20
JP2016-107997 2016-05-31
JP2016107997 2016-05-31
JP2016-111569 2016-06-03
JP2016111569A JP2017215304A (ja) 2015-12-16 2016-06-03 カラム

Publications (1)

Publication Number Publication Date
WO2017104747A1 true WO2017104747A1 (fr) 2017-06-22

Family

ID=59056591

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2016/087375 WO2017104747A1 (fr) 2015-12-16 2016-12-15 Colonne

Country Status (1)

Country Link
WO (1) WO2017104747A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018212165A1 (fr) * 2017-05-16 2018-11-22 株式会社ダイセル Tube de colonne pour chromatographie, et colonne pour chromatographie l'employant

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04503408A (ja) * 1989-02-21 1992-06-18 イーストマン コダック カンパニー 非多孔質単分散ポリマー充填物質を含む高速アフィニティクロマトグラフカラム
JPH07209250A (ja) * 1983-10-19 1995-08-11 Hewlett Packard Co <Hp> 電気化学検出器
JPH09119924A (ja) * 1995-08-01 1997-05-06 Hewlett Packard Co <Hp> クロマトグラフィー用分離カラム

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07209250A (ja) * 1983-10-19 1995-08-11 Hewlett Packard Co <Hp> 電気化学検出器
JPH04503408A (ja) * 1989-02-21 1992-06-18 イーストマン コダック カンパニー 非多孔質単分散ポリマー充填物質を含む高速アフィニティクロマトグラフカラム
JPH09119924A (ja) * 1995-08-01 1997-05-06 Hewlett Packard Co <Hp> クロマトグラフィー用分離カラム

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018212165A1 (fr) * 2017-05-16 2018-11-22 株式会社ダイセル Tube de colonne pour chromatographie, et colonne pour chromatographie l'employant
JPWO2018212165A1 (ja) * 2017-05-16 2020-03-26 株式会社ダイセル クロマトグラフィー用カラム管及びそれを用いたクロマトグラフィー用カラム
JP7041132B2 (ja) 2017-05-16 2022-03-23 株式会社ダイセル クロマトグラフィー用カラム管及びそれを用いたクロマトグラフィー用カラム

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