JP2021131235A - Liquid chromatography adapter - Google Patents
Liquid chromatography adapter Download PDFInfo
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- JP2021131235A JP2021131235A JP2020025123A JP2020025123A JP2021131235A JP 2021131235 A JP2021131235 A JP 2021131235A JP 2020025123 A JP2020025123 A JP 2020025123A JP 2020025123 A JP2020025123 A JP 2020025123A JP 2021131235 A JP2021131235 A JP 2021131235A
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- column
- adapter
- main body
- seal member
- liquid chromatography
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- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 8
- 229920002530 polyetherether ketone Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polychlorotrifluoroethylene Polymers 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、迅速かつ簡便に精度よくカラムを着脱可能にする液体クロマトグラフィー用のアダプターに関するものである。 The present invention relates to an adapter for liquid chromatography that enables quick, convenient, and accurate attachment and detachment of a column.
液体クロマトグラフィーを原理とする分析装置において、カラムと配管との接続はフェラルと圧縮ねじからなる構成が一般的であるが、この構成では汎用性は高いものの、接続作業が確実かつ簡便に行えず、個人差が生じやすい。 In an analyzer based on liquid chromatography, the connection between a column and a pipe is generally composed of a ferrule and a compression screw. Although this configuration is highly versatile, the connection work cannot be performed reliably and easily. , Individual differences are likely to occur.
特許文献１では、装置への取付け・取外しを簡便におこなうことを目的とした液体クロマトグラフィー用カラムとして、カラムボディ閉止機能を有するエンドキャップと、配管接続機能を有するジョイント部材とに分割し、シール部材を介してこれらを当接し、ケースに対する蓋部材の着脱作業だけで、エンドキャップ付きのカラムボディの交換（取付け・取外し）を可能とする構造が提案されている。 In Patent Document 1, as a column for liquid chromatography intended to be easily attached to and detached from an apparatus, it is divided into an end cap having a column body closing function and a joint member having a pipe connecting function, and sealed. A structure has been proposed in which these are brought into contact with each other via members, and the column body with an end cap can be replaced (attached / removed) only by attaching / detaching the lid member to / from the case.
本発明の課題は、迅速かつ簡便に精度よくカラムを装置に取り付けるためのアダプターを提供することにある。 An object of the present invention is to provide an adapter for mounting a column to an apparatus quickly, easily and accurately.
前記課題を解決するためになされた本発明は、以下の発明を包含する：
すなわち本発明の一態様は、
本体と、前記本体に装入されたシール部材と、を含んでなる、液体クロマトグラフィー用カラムと溶離液の送液配管とを接続するためのアダプターであって、前記シール部材に、前記液体クロマトグラフィー用カラムの開口部及び前記送液配管の開口部と当接可能な流路を備えていることを特徴とする。
The present invention made to solve the above problems includes the following inventions:
That is, one aspect of the present invention is
An adapter for connecting a column for liquid chromatography and a liquid feeding pipe for eluent, which comprises a main body and a seal member charged in the main body, and the liquid chromatograph is attached to the seal member. It is characterized by including an opening of a chromatography column and a flow path capable of contacting the opening of the liquid feeding pipe.
本発明は、カラムと配管を迅速かつ簡便に精度よく接続することができる。 According to the present invention, a column and a pipe can be connected quickly, easily and accurately.
以下に本発明を詳細に説明するが、本発明はこの態様に限定されるものではない。 The present invention will be described in detail below, but the present invention is not limited to this aspect.
本体とは、アダプターからシール部材を取り除いたものを指し、外観は略円柱体又は凸型円柱形であり、内部は内径の異なる貫通孔がつながっている。すなわち、円筒形状の一種である。なお、前記貫通孔の一部がシール部材の装入部を構成する。 The main body refers to an adapter from which the sealing member has been removed, and has a substantially cylindrical or convex cylindrical appearance, and through holes having different inner diameters are connected to the inside. That is, it is a kind of cylindrical shape. A part of the through hole constitutes a charging portion of the seal member.
また、本体はカラムエンドと螺合可能なネジ部を備えていることが好ましい。一般に雌ネジ山を形成するカラムエンドとの螺合によりカラムに接続する場合は、本体の外周に雄ネジ山を有する構造とすることが例示できる。さらに、本体はナット部を備えていてもよく、その形状としては、スパナやレンチ等の工具を用いてカラムアダプターをカラムに着脱が可能な二面幅、四角又は六角などが例示できる。 Further, it is preferable that the main body is provided with a screw portion that can be screwed with the column end. Generally, when connecting to a column by screwing with a column end forming a female thread, a structure having a male thread on the outer circumference of the main body can be exemplified. Further, the main body may be provided with a nut portion, and the shape thereof may be exemplified by a width across flats, a square or a hexagon in which a column adapter can be attached to and detached from a column using a tool such as a spanner or a wrench.
また、本体は継手を介して送液配管と接合可能な篏合部を備えていることが好ましい。継手は、一般的に用いられるフェラルなどが例示でき、圧縮ネジ式の配管先端部に螺合により装着でき、本体内周と当接可能な大きさ・形状であれば問題ない。本体内周と継手が当接するように、本体内周に嵌合部を設けておく。すなわち、嵌合部の形状は継手の形状によって決まるが、略円錐台形状などが好適である。アダプターと嵌合接続する方法は、例えばカラム載置部と、カラムの両方向に対向配置するクランプ部と、及び回転レバー方式による加圧部とをベース部に設けたカラム接続器等により好適に対応することができる。 Further, it is preferable that the main body is provided with a fitting portion that can be joined to the liquid feed pipe via a joint. As the joint, a commonly used ferrule or the like can be exemplified, and there is no problem as long as it can be attached to the tip of a compression screw type pipe by screwing and has a size and shape that allows contact with the inner circumference of the main body. A fitting portion is provided on the inner circumference of the main body so that the inner circumference of the main body and the joint come into contact with each other. That is, the shape of the fitting portion is determined by the shape of the joint, but a substantially truncated cone shape or the like is preferable. The method of fitting and connecting to the adapter is preferably supported by, for example, a column connector in which a column mounting portion, a clamp portion arranged to face each other in both directions of the column, and a pressurizing portion by a rotary lever method are provided on the base portion. can do.
本体の材質はＳＵＳが好ましいが、例えば対象試料が金属フリーの環境下で測定する必要があるなど接液部にＳＵＳが使用できない場合は、カラム及び配管の材質に合わせた樹脂、またはＳＵＳに樹脂を被覆したものことも可能である。 The material of the main body is preferably SUS, but if SUS cannot be used for the wetted parts, for example, when the target sample needs to be measured in a metal-free environment, resin suitable for the material of the column and piping, or resin for SUS. It is also possible to cover it with.
シール部材の材質は、液体クロマトグラフィー用カラムの開口部及び送液配管の開口部との加圧接面において良好なシール性が発揮できるようにポリエーテルエーテルケトン（ＰＥＥＫ）、ポリイミド（ＰＩ）、ポリアセタール（ＰＯＭ）、ポリクロロトリフルオロエチレン（ＰＣＴＦＥ）等の弾性と高い圧縮強度を示す樹脂、又は前記樹脂をベースにガラス、炭素等の強化材を添加したものが好適に使用でき、特にポリエーテルエーテルケトンが好ましい。 The material of the sealing member is polyetheretherketone (PEEK), polyimide (PI), polyacetal so that good sealing performance can be exhibited at the pressure contact surface with the opening of the liquid chromatography column and the opening of the liquid feeding pipe. A resin exhibiting elasticity and high compressive strength such as (POM) and polychlorotrifluoroethylene (PCTFE), or a resin based on the resin to which a reinforcing material such as glass or carbon is added can be preferably used, and in particular, polyetherether. Ketone is preferred.
シール部材の形状は、略円柱体、略円錐体、略円錐台、略立方体、略直方体等の中心軸線に溶離液用の流路を設けたものが例示できる。液体クロマトグラフィー用カラムの開口部及び送液配管の開口部との当接面の形状は、流路の開口部周辺の樹脂が加圧圧力により変形して効率よく当接面をシールすることができるようにシール部材の開口部（流路）を頂点とする略錐体形状又は略球面形状に樹脂を盛るとシール性が向上する点において好ましい。つぶし代としては、シール部材全長の３％〜１０％であることが好ましい。 Examples of the shape of the sealing member include those in which a flow path for an eluent is provided on the central axis of a substantially cylindrical body, a substantially conical body, a substantially truncated cone, a substantially cubic body, a substantially rectangular parallelepiped, or the like. The shape of the contact surface between the opening of the liquid chromatography column and the opening of the liquid feed pipe is such that the resin around the opening of the flow path is deformed by the pressurized pressure to efficiently seal the contact surface. It is preferable to pour the resin into a substantially pyramidal shape or a substantially spherical shape having the opening (flow path) of the sealing member as the apex so that the sealing property is improved. The crushing allowance is preferably 3% to 10% of the total length of the seal member.
さらにシール部材に設けた流路は、その中心軸がカラムの中心軸の延長線と一致するように設けることが、溶離液がスムーズに流れる点において好ましい。シール部材はカラムと接続する側から装入して位置決めしても、反対側から装入して位置決めしてもよく、シール部材及びアダプターの形状に合わせて適宜選択すれば問題はない。 Further, it is preferable that the flow path provided in the seal member is provided so that the central axis thereof coincides with the extension line of the central axis of the column from the viewpoint of smooth flow of the eluent. The seal member may be charged and positioned from the side connected to the column, or may be charged and positioned from the opposite side, and there is no problem as long as it is appropriately selected according to the shape of the seal member and the adapter.
以下、実施例等を用いて本発明をさらに詳細に説明するが、本発明の態様はこれらに限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to Examples and the like, but the embodiments of the present invention are not limited thereto.
（実施例１）
図１は本発明のアダプターの一態様を示す断面図である。
シール部材１０２は直径の異なる略円柱体を軸方向に直列に重ねた形状（凸型円柱形）に一体成形したブロックとし、中心軸上に溶離液用の流路１０３を設けた。シール部材１０２の配管先端部又はカラムとの当接面の形状は、流路の開口部を頂点とする略円錐形になるよう樹脂を盛り、加圧によるつぶし代を設けた。材質はＰＥＥＫとした。
本体１０１はＳＵＳ製とし、継手３０３と当接可能に嵌合するように嵌合部１０６を設けた。シール部材を装入して位置決めが可能な凹部をカラム接合側に設けた。また、雌ネジ山４０２を形成したカラムエンドとの螺合による接続が可能なように、本体外周に雄ネジ山１０７を形成した。さらに、スパナを用いてアダプターをカラム４０１に接続するために外周に六角形状のナット部１０８を形成した。
(Example 1)
FIG. 1 is a cross-sectional view showing one aspect of the adapter of the present invention.
The
The
（実施例２）
図３は本発明のアダプターの別態様を示す断面図である。
シール部材２０２は液体クロマトグラフィー用のＰＥＥＫ配管（チューブ形）を高精度カットして作製した。本体２０１はＳＵＳ製とし、継手３０３と当接可能に嵌合するように嵌合部２０６を設けた。シール部材２０２を装入して位置決めが可能な貫通部をカラム接合側に設けた。また、雌ネジ山４０２を形成したカラムエンドとの螺合による接続が可能なように、本体外周に雄ネジ山２０７を形成した。さらに、スパナを用いてアダプターをカラム４０１に接続するために外周に六角形状のナット部２０８を形成した。
(Example 2)
FIG. 3 is a cross-sectional view showing another aspect of the adapter of the present invention.
The
（実施例３）
以下の３種類のシール部材を作製した。
シール部材１：凸型円柱形、ＰＥＥＫ製、つぶし代０．２ｍｍ、全長５．７ｍｍ
シール部材２：凸型円柱形、ＰＥＥＫ製、つぶし代０．４ｍｍ、全長５．９ｍｍ
シール部材３：チューブ形、ＰＥＥＫ製、つぶし代０．５ｍｍ、全長６．０ｍｍ
なお、シール部材の流路直径はいずれも０．２５ｍｍとした。
シール部材１又はシール部材２を用いて実施例１に記載のアダプターを作製し、シール部材３を用いて実施例２に記載のアダプターを作製して耐圧試験を行った。
(Example 3)
The following three types of sealing members were produced.
Seal member 1: Convex cylindrical shape, made of PEEK, crushing allowance 0.2 mm, total length 5.7 mm
Seal member 2: Convex cylindrical shape, made of PEEK, crushing allowance 0.4 mm, total length 5.9 mm
Seal member 3: Tube type, made of PEEK, crushing allowance 0.5 mm, total length 6.0 mm
The flow path diameter of the seal member was set to 0.25 mm.
The adapter described in Example 1 was produced using the seal member 1 or the seal member 2, and the adapter described in Example 2 was produced using the seal member 3, and a pressure resistance test was performed.
カラムサイズが内径３．５ｍｍ、長さが１０ｍｍ、１５ｍｍ、２０ｍｍ、及び２５ｍｍの４本のカラムを用意し、カラム充填剤ＴＳＫｇｅｌ ＤＥＡＥ−ＮＰＲ（東ソー株式会社、 粒子径２．５μｍ）を充填した。充填後のカラムの入口側及び出口側にアダプターを接続し、送液ポンプはＤＰ−８０２０（東ソー株式会社）を使用して蒸留水を移動相として送液した（図２、４参照）。
上記４本のカラムを使用した際のシステム圧力がそれぞれ５〜１０ＭＰａ、１０〜１５ＭＰａ、１５〜２０ＭＰａ、及び２０〜２５ＭＰａになるように送液流量を調整し、１０分間送液した。送液開始時のシステム圧力と１０分経過後のシステム圧力について表示圧力値を記録し、圧力降下を確認した（表１参照）。その結果、いずれも圧力降下は０．１ＭＰａ以下であり、液漏れは発生しなかった。また、すべての試験終了後にシール部材の全長を測定すると、試験後は試験前と比較して、シール部材の全長が短くなっており、シール部材が軸方向に圧縮変形していることを確認した（表２参照）。
Four columns having a column size of 3.5 mm in inner diameter and lengths of 10 mm, 15 mm, 20 mm, and 25 mm were prepared and filled with the column packing material TSKgel DEAE-NPR (Tosoh Corporation, particle size 2.5 μm). Adapters were connected to the inlet side and outlet side of the column after filling, and the liquid feed pump used DP-8020 (Tosoh Corporation) to feed distilled water as a mobile phase (see FIGS. 2 and 4).
The liquid feed flow rate was adjusted so that the system pressures when the above four columns were used were 5 to 10 MPa, 10 to 15 MPa, 15 to 20 MPa, and 20 to 25 MPa, respectively, and the liquid was fed for 10 minutes. The displayed pressure values were recorded for the system pressure at the start of liquid transfer and the system pressure after 10 minutes, and the pressure drop was confirmed (see Table 1). As a result, the pressure drop was 0.1 MPa or less in each case, and no liquid leakage occurred. In addition, when the total length of the seal member was measured after all the tests were completed, it was confirmed that the total length of the seal member was shorter after the test than before the test, and that the seal member was compressionally deformed in the axial direction. (See Table 2).
１０１、２０１：本体
１０２、２０２：シール部材
１０３、２０３：流路
１０６，２０６：嵌合部
１０７、２０７：雄ネジ山
１０８、２０８：ナット部
３０１ ：圧縮ネジ
３０２ ：送液配管
３０３ ：継手
４０１ ：カラム
４０２ ：雌ネジ山
４０３ ：カラムフィルター
４０４ ：カラムエンド
101, 201:
Claims (6)
前記本体に装入されたシール部材と、
を含んでなる、液体クロマトグラフィー用カラムと溶離液の送液配管とを接続するためのアダプターであって、
前記シール部材に、前記液体クロマトグラフィー用カラムの開口部及び前記送液配管の開口部と当接可能な流路を備えていることを特徴とする前記アダプター。 With the main body
The seal member charged in the main body and
An adapter for connecting a liquid chromatography column and an eluent feed pipe, which comprises the above.
The adapter characterized in that the sealing member includes an opening of the liquid chromatography column and a flow path capable of contacting the opening of the liquid feeding pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2020025123A JP7388232B2 (en) | 2020-02-18 | 2020-02-18 | Adapter for liquid chromatography |
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| JP2020025123A JP7388232B2 (en) | 2020-02-18 | 2020-02-18 | Adapter for liquid chromatography |
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| JP2021131235A true JP2021131235A (en) | 2021-09-09 |
| JP7388232B2 JP7388232B2 (en) | 2023-11-29 |
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| JP4972329B2 (en) | 2006-03-27 | 2012-07-11 | 株式会社日立ハイテクノロジーズ | High performance liquid chromatograph column and high performance liquid chromatograph |
| GB2478449B (en) | 2008-12-23 | 2013-01-30 | Optimize Tech Inc | Assembly for placing an insert into communication with an analytical chemical instrument |
| NO2975398T3 (en) | 2013-03-11 | 2018-07-21 | ||
| DE112016006724T5 (en) | 2016-05-17 | 2018-12-27 | Hitachi High-Technologies Corporation | COLUMN CONNECTION DEVICE, CONNECTION METHOD AND ANALYSIS SYSTEM |
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