JP2004060513A - Liquid delivery pump for liquid chromatograph - Google Patents

Liquid delivery pump for liquid chromatograph Download PDF

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Publication number
JP2004060513A
JP2004060513A JP2002219261A JP2002219261A JP2004060513A JP 2004060513 A JP2004060513 A JP 2004060513A JP 2002219261 A JP2002219261 A JP 2002219261A JP 2002219261 A JP2002219261 A JP 2002219261A JP 2004060513 A JP2004060513 A JP 2004060513A
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JP
Japan
Prior art keywords
plunger
working fluid
liquid
seal
core
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
JP2002219261A
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Japanese (ja)
Inventor
Ryutaro Oda
小田 竜太郎
Yousuke Iwata
岩田 庸助
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
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 Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP2002219261A priority Critical patent/JP2004060513A/en
Publication of JP2004060513A publication Critical patent/JP2004060513A/en
Pending legal-status Critical Current

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Abstract

<P>PROBLEM TO BE SOLVED: To provide a liquid delivery pump capable of preventing salts etc. from being produced or precipitated at/to the plunger surfaces and also its seal from wearing or damaging resulting therefrom even in case a working fluid delivered contains solids such as a buffer solution etc. <P>SOLUTION: A core 21 surface of a coat plunger 9C is coated with a coating film 20, for example DLC, of different material from the core 21, for example sapphire. This allows preventing salts etc. from being produced or precipitated at/to the surfaces of the plunger 9C and also the seal from wearing or damaging resulting therefrom even in case the working fluid delivered contains solids such as a buffer solution etc., and it is possible to establish a stable operation for a long time and improve the man-hours for maintenance operations. <P>COPYRIGHT: (C)2004,JPO

Description

【0001】
【発明の属する技術分野】
本発明は、プランジャを内蔵しこのプランジャを往復駆動させて送液する液体クロマトグラフ用送液ポンプに関する。
【0002】
【従来の技術】
従来より、液体クロマトグラフ用送液ポンプのポンプ機構としては、主にプランジャ方式のポンプが多く採用されている。プランジャポンプの主要部品であるプランジャの材質に求められる特性としては耐薬品性があること、プランジャと摺動するシールの摩耗を抑えるためプランジャ表面を平滑に製作できることが挙げられる。この特性を満たす材料として、サファイア、ジルコニアセラミックが多く使用されている。
【0003】
以下、図2(a)および図2(b)にしたがって従来のプランジャポンプ(以下、場合によりポンプと呼ぶ)の構造を説明する。図2(b)に示すモータ14の回転軸、カム軸7およびカム12が回転する。カム12には図2(a)に示すカムフォロワ13が外接しており、カム12の回転によってカムフォロワ13も回転する。カムフォロワ13と滑動するフォロワ軸3は円筒形状のクロスヘッド6と固着されているので、カム12の回転はポンプヘッド4に滑合しているクロスヘッド6の直線往復運動に変換される。クロスヘッド6はバネ5により常に図の右方向に付勢されているのでカム12とカムフォロワ13は常に係合を保っている。クロスヘッド6には円筒形状のプランジャ9が軸芯上に延設されており、プランジャ9の往復運動によって作動流体室Vの容積が周期的に増減する。逆止弁1および逆止弁8は、送液される作動流体(図示せず)の流れの方向を図2(a)の下方から上方のみに限定するために挿入されている。作動流体のクロスヘッド6方向への漏洩はプランジャ9を囲む円環形状のシール11により防止される。
【0004】
ポンプヘッド4とシール11とプランジャ9で囲まれた作動流体室Vの容積がプランジャ9の右方への移動によって増大する期間に、作動流体は図の下方から作動流体室Vに吸入される。この期間は図の上方からの作動流体の吸入は逆止弁1により防止されている。容積が減少する期間は図の下方への作動流体の流出が逆止弁8により防止されるので、作動流体は図の上方に逆止弁1を通過してポンプから吐出する。
【0005】
作動流体が緩衝液等の固形物を溶かしたものである場合には、ある期間の使用によってその塩等がプランジャ9の表面に析出しシール11との円滑な滑動を阻害するので、洗浄流路2には定期的に蒸留水など塩等を溶解する洗浄液を流すかまたは洗浄液を封入して、塩等を除去し円滑な滑動を回復または維持する必要がある。洗浄液の外部への漏洩はシール10とシール11により防止される。
【0006】
【発明が解決しようとする課題】
従来の液体クロマトグラフ用送液ポンプは以上のとおりであるが、従来のプランジャ9の主たる材質として使用されているサファイアはジルコニアセラミックと比較して平滑性に優れており、一般的にはシール11の寿命はジルコニアセラミックの場合と比較して長い。しかしながら、作動流体が緩衝液等の固形物を溶かしたものである場合には、プランジャ9の材質としてサファイアを使用した時はジルコニアセラミックスを使用した時よりもシール11の寿命が短く、プランジャ表面に固体の塩等がサファイア上に強固に析出し、洗浄流路2に繰り返し洗浄液を注入して塩等の洗浄を行っても洗浄液の供給が不十分なプランジャ9とシール11の界面部分からプランジャ9の表面に固体の塩等が析出し、次第にプランジャ9とシール11の摩擦が増大してシール11の摩耗・損傷を生じ、その寿命を短縮していた。また塩等の発生はジルコニアセラミックについてもサファイアよりは少ないとはいえ、避けることができない。
【0007】
本発明はこのような問題点を解決する液体クロマトグラフ用送液ポンプを提供することを目的とするものである。
【0008】
【課題を解決するための手段】
本発明の液体クロマトグラフ用送液ポンプは、上記課題を解決するために、プランジャの心材の表面を心材とは異なる材質の被覆膜で被覆するものである。この被覆によって、プランジャは平滑性を維持しつつ化学的な安定性を確保することができる。
【0009】
【発明の実施の形態】
本発明の液体クロマトグラフ用送液ポンプを図1(a)および図1(b)にしたがって説明する。カム軸7の周囲を回転するカム12の回転運動はカムフォロワ13の回転およびクロスヘッド6の直線往復運動を介してクロスヘッド6と固着しているコートプランジャ9Cの直線往復運動を生じ、作動流体室Vの容積を周期的に増減させる。作動流体室Vを経由する作動流体の流れの方向は逆止弁8および逆止弁1により図の下方から上方へのみ行われるので、作動流体は作動流体室Vの容積が増大する期間は逆止弁8を通過して下方より作動流体室Vへ導入され、作動流体室Vの容積が減少する期間は逆止弁1を通過して上方へ吐出される。
【0010】
本発明のプランジャポンプにおいては図1(b)に示すごとく、コートプランジャ9Cの心材21の表面を心材21とは異なる材質からなる被覆膜20で被覆したコートプランジャ9Cを内蔵する。たとえば心材21としてサファイアを使用し、その表面を平滑に研磨した後、被覆膜20としてDLC(DiamondLike Carbon、ダイヤモンド状カーボン)を被覆する。DLCはサファイアに比較して化学的に安定であり、作動流体に侵されたり、作動流体に含まれる物質と反応したり、作動流体中の塩等を析出したりする傾向がはるかに小さい。なお、図1において図2と同一の番号または記号を付する部品は図2と同一である。
【0011】
本発明のプランジャポンプについては上記の実施例に限定されるものではなく、種々の変形実施例を挙げることができる。たとえばコートプランジャ9Cの心材21として超硬合金を使用したもの、被覆膜20としてDLC膜に変えてジルコニアセラミックの薄膜をPVD法(Physical Vapor Deposition法)で作成したもの、またはそれらを組み合わせたものなど、種々の心材21および被覆膜20を使用することができる。すなわちジルコニアセラミックは単体ではサファイアに比較して表面の平滑性に劣っているが、被覆膜20として使用すれば、平滑性はサファイアに依存し、化学的安定性はジルコニアセラミックに依存するコートプランジャ9Cを実現することができる。本発明はコートプランジャ9Cの心材21が被覆膜20の材質と異なるものであればよく、心材21の材質、被覆膜20の材質、被覆膜20の作成方法は限定されない。また図1の実施例ではコートプランジャ9Cの端面は被覆されていないが、端面を含めて被覆膜20で被覆しても良い。本発明はこれらをすべて包含する。
【0012】
【発明の効果】
本発明は以上詳述したとおりであるから、プランジャの心材とは異なる材質の被覆膜で心材の表面を被覆したプランジャの内蔵によって、心材の平滑性を保ったまま化学的に安定なプランジャ表面を提供でき、作動流体が緩衝液等の固形物を含む場合でもプランジャの表面への塩等の発生・析出およびそれに起因するシールの摩耗・損傷を防止し、長期間の安定な作動と保守工数の改善を実現した液体クロマトグラフ用送液ポンプを実現することが可能になる。
【図面の簡単な説明】
【図1】(a)は本発明のプランジャポンプの構造を示す断面図、(b)はプランジャ部の構造を示す断面図である。
【図2】(a)は従来のプランジャポンプの構造を示す断面図、(b)はカムとモータの接続を示す斜視図である。
【符号の説明】
6…クロスヘッド
9…プランジャ
10…シール
11…シール
9C…コートプランジャ
20…被覆膜
21…心材
V…作動流体室
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a liquid chromatography pump for a liquid chromatograph, which has a built-in plunger and reciprocates the plunger to feed liquid.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, as a pump mechanism of a liquid chromatograph liquid transfer pump, a plunger type pump has been mainly used in many cases. Characteristics required for the material of the plunger, which is a main component of the plunger pump, include chemical resistance and the ability to produce a smooth plunger surface to suppress wear of a seal sliding with the plunger. Sapphire and zirconia ceramics are often used as materials satisfying this property.
[0003]
Hereinafter, the structure of a conventional plunger pump (hereinafter, sometimes referred to as a pump) will be described with reference to FIGS. 2A and 2B. The rotation shaft of the motor 14, the camshaft 7, and the cam 12 shown in FIG. 2B rotate. A cam follower 13 shown in FIG. 2A circumscribes the cam 12, and the rotation of the cam 12 causes the cam follower 13 to rotate. Since the cam follower 13 and the follower shaft 3 that slides are fixed to the cylindrical crosshead 6, the rotation of the cam 12 is converted into a linear reciprocating motion of the crosshead 6 that slides on the pump head 4. Since the crosshead 6 is always urged rightward in the figure by the spring 5, the cam 12 and the cam follower 13 always maintain engagement. A cylindrical plunger 9 extends on the axis of the crosshead 6, and the volume of the working fluid chamber V periodically increases and decreases due to the reciprocating motion of the plunger 9. The check valve 1 and the check valve 8 are inserted in order to limit the flow direction of the working fluid (not shown) to be fed from below to above in FIG. Leakage of the working fluid in the direction of the crosshead 6 is prevented by the annular seal 11 surrounding the plunger 9.
[0004]
During a period in which the volume of the working fluid chamber V surrounded by the pump head 4, the seal 11, and the plunger 9 increases due to the rightward movement of the plunger 9, the working fluid is sucked into the working fluid chamber V from below in the figure. During this period, the suction of the working fluid from above in the drawing is prevented by the check valve 1. Since the check valve 8 prevents the outflow of the working fluid downward in the figure during the period in which the volume is reduced, the working fluid is discharged from the pump through the check valve 1 above the figure.
[0005]
When the working fluid is a solution in which a solid such as a buffer solution is dissolved, the salt or the like precipitates on the surface of the plunger 9 during use for a certain period of time and hinders smooth sliding with the seal 11. In step 2, it is necessary to periodically flow a washing solution such as distilled water for dissolving salts or the like, or to enclose a washing solution to remove salts and the like to recover or maintain smooth sliding. The leakage of the cleaning liquid to the outside is prevented by the seals 10 and 11.
[0006]
[Problems to be solved by the invention]
The conventional liquid chromatograph pump is as described above, but sapphire used as a main material of the conventional plunger 9 is superior in smoothness to zirconia ceramics, and generally has a seal 11. Has a longer life than zirconia ceramics. However, when the working fluid is a solution in which a solid such as a buffer solution is dissolved, the life of the seal 11 is shorter when sapphire is used as the material of the plunger 9 than when zirconia ceramics is used. The solid salt or the like strongly precipitates on the sapphire, and even if the washing liquid is repeatedly injected into the washing flow path 2 to wash the salt or the like, the supply of the washing liquid is insufficient. Solids and the like are deposited on the surface of the seal 11 and the friction between the plunger 9 and the seal 11 gradually increases, causing wear and damage of the seal 11 and shortening its life. The generation of salts and the like cannot be avoided in zirconia ceramics, though it is less than in sapphire.
[0007]
An object of the present invention is to provide a liquid chromatography pump for solving such a problem.
[0008]
[Means for Solving the Problems]
In order to solve the above-described problems, the liquid pump for liquid chromatography of the present invention covers the surface of the core of the plunger with a coating film made of a material different from that of the core. With this coating, the plunger can ensure chemical stability while maintaining smoothness.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
The liquid pump for liquid chromatography of the present invention will be described with reference to FIGS. 1 (a) and 1 (b). Rotational movement of the cam 12 rotating around the cam shaft 7 causes linear reciprocating movement of the coat plunger 9C fixed to the crosshead 6 through rotation of the cam follower 13 and linear reciprocating movement of the crosshead 6. The volume of V is periodically increased or decreased. Since the direction of the flow of the working fluid through the working fluid chamber V is performed only from the bottom to the top of the drawing by the check valve 8 and the check valve 1, the working fluid is reversed during the period in which the volume of the working fluid chamber V increases. After passing through the stop valve 8, it is introduced into the working fluid chamber V from below, and is discharged upward through the check valve 1 during a period in which the volume of the working fluid chamber V decreases.
[0010]
As shown in FIG. 1B, the plunger pump of the present invention incorporates a coat plunger 9C in which the surface of the core 21 of the coat plunger 9C is covered with a coating film 20 made of a material different from that of the core 21. For example, sapphire is used as the core material 21 and its surface is polished smoothly, and then the coating film 20 is coated with DLC (DiamondLike Carbon, diamond-like carbon). DLC is chemically more stable than sapphire, and has a much lower tendency to be attacked by the working fluid, to react with substances contained in the working fluid, and to precipitate salts and the like in the working fluid. In FIG. 1, components denoted by the same reference numerals or symbols as those in FIG. 2 are the same as those in FIG.
[0011]
The plunger pump of the present invention is not limited to the above embodiment, and various modified embodiments can be cited. For example, the core material 21 of the coat plunger 9C is made of a cemented carbide, the coating film 20 is made of a zirconia ceramic thin film instead of the DLC film, and the zirconia ceramic thin film is made by PVD (Physical Vapor Deposition) method, or a combination thereof. For example, various core materials 21 and coating films 20 can be used. In other words, zirconia ceramics alone have poor surface smoothness as compared to sapphire, but when used as a coating film 20, a coat plunger whose smoothness depends on sapphire and whose chemical stability depends on zirconia ceramics. 9C can be realized. In the present invention, the core material 21 of the coat plunger 9C may be different from the material of the coating film 20, and the material of the core material 21, the material of the coating film 20, and the method of forming the coating film 20 are not limited. In the embodiment of FIG. 1, the end face of the coat plunger 9C is not covered, but may be covered with the covering film 20 including the end face. The present invention includes all of these.
[0012]
【The invention's effect】
Since the present invention has been described in detail above, by incorporating a plunger in which the surface of the core is covered with a coating film different from the core of the plunger, a chemically stable plunger surface is maintained while maintaining the smoothness of the core. To prevent the generation and precipitation of salts and the like on the surface of the plunger and the abrasion and damage of the seal due to it even when the working fluid contains solids such as buffer solution, thus ensuring long-term stable operation and maintenance man-hours. It is possible to realize a liquid chromatography pump for liquid chromatography that has improved the above.
[Brief description of the drawings]
FIG. 1A is a sectional view showing a structure of a plunger pump of the present invention, and FIG. 1B is a sectional view showing a structure of a plunger portion.
FIG. 2A is a sectional view showing a structure of a conventional plunger pump, and FIG. 2B is a perspective view showing a connection between a cam and a motor.
[Explanation of symbols]
6 Crosshead 9 Plunger 10 Seal 11 Seal 9C Coat plunger 20 Coating film 21 Core material V Working fluid chamber

Claims (3)

プランジャの心材の表面を心材とは異なる材質の被覆膜で被覆したプランジャを内蔵することを特徴とする液体クロマトグラフ用送液ポンプ。A liquid pump for liquid chromatography, comprising a built-in plunger in which the surface of a core material of a plunger is coated with a coating film made of a material different from that of the core material. プランジャの心材を単結晶で構成したことを特徴とする請求項1記載の液体クロマトグラフ用送液ポンプ。2. The liquid pump according to claim 1, wherein the core material of the plunger is made of a single crystal. プランジャの心材を超硬合金で構成したことを特徴とする請求項1記載の液体クロマトグラフ用送液ポンプ。The liquid pump for liquid chromatography according to claim 1, wherein the core material of the plunger is made of a cemented carbide.
JP2002219261A 2002-07-29 2002-07-29 Liquid delivery pump for liquid chromatograph Pending JP2004060513A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
JP2002219261A JP2004060513A (en) 2002-07-29 2002-07-29 Liquid delivery pump for liquid chromatograph

Publications (1)

Publication Number Publication Date
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Family

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Country Status (1)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015183139A3 (en) * 2014-05-30 2016-01-21 Ооо "Фармасапфир" Positive displacement hydraulic device for pumping and/or dosing liquids
EP2939810A4 (en) * 2012-12-27 2016-08-24 Obschestvo S Ogranichennoy Otvetstvennostyu Farmasapfir Method for processing cylindrical surfaces of sapphire parts, a sapphire piston pair and a metering pump on the basis thereof
CN108180136A (en) * 2017-12-29 2018-06-19 浙江福立分析仪器股份有限公司 A kind of infusion pump of liquid chromatograph and the method for reducing sealing surface wear
JPWO2021132604A1 (en) * 2019-12-27 2021-07-01

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2939810A4 (en) * 2012-12-27 2016-08-24 Obschestvo S Ogranichennoy Otvetstvennostyu Farmasapfir Method for processing cylindrical surfaces of sapphire parts, a sapphire piston pair and a metering pump on the basis thereof
WO2015183139A3 (en) * 2014-05-30 2016-01-21 Ооо "Фармасапфир" Positive displacement hydraulic device for pumping and/or dosing liquids
RU2578373C2 (en) * 2014-05-30 2016-03-27 Виталий Алексеевич САВЕНКОВ Hydraulic device of volumetric displacement for pumping and/or proportioning liquids
CN108180136A (en) * 2017-12-29 2018-06-19 浙江福立分析仪器股份有限公司 A kind of infusion pump of liquid chromatograph and the method for reducing sealing surface wear
JPWO2021132604A1 (en) * 2019-12-27 2021-07-01
WO2021132604A1 (en) * 2019-12-27 2021-07-01 京セラ株式会社 Plunger, pump, and liquid analysis device
CN114846241A (en) * 2019-12-27 2022-08-02 京瓷株式会社 Plunger, pump, and liquid analyzer

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