JP2000039428A - Column thermostatic chamber - Google Patents

Column thermostatic chamber

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Publication number
JP2000039428A
JP2000039428A JP10204757A JP20475798A JP2000039428A JP 2000039428 A JP2000039428 A JP 2000039428A JP 10204757 A JP10204757 A JP 10204757A JP 20475798 A JP20475798 A JP 20475798A JP 2000039428 A JP2000039428 A JP 2000039428A
Authority
JP
Japan
Prior art keywords
column
resin
thermally
temperature
thermally conductive
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.)
Granted
Application number
JP10204757A
Other languages
Japanese (ja)
Other versions
JP3982071B2 (en
Inventor
Norio Hirachi
教郎 平地
Hidechika Hayashi
秀知佳 林
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.)
Tosoh Corp
Original Assignee
Tosoh 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 Tosoh Corp filed Critical Tosoh Corp
Priority to JP20475798A priority Critical patent/JP3982071B2/en
Publication of JP2000039428A publication Critical patent/JP2000039428A/en
Application granted granted Critical
Publication of JP3982071B2 publication Critical patent/JP3982071B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To easily maintain the desorption or the like of a column and to accurately control temperature even in the column with various kinds of diversified outer shapes and outer diameters by providing a thermally conductive resin for thermally connecting a column being accommodated inside and an enclosure. SOLUTION: An enclosure 1 accommodates a column 7 inside and is divided into a body A and a lid B to facilitate the maintenance, for example, for exchanging the accommodated column 7. Also, a heat generation source (cooling source) 4 such as a heater or a thermoelectric element is arranged while it is thermally connected, and a temperature sensor 5 for controlling temperature is mounted. Then, a thermally conductive resin 6 for thermally connecting at least one portion of the column 7 and the enclosure 1 is equipped. Although there is no limitation as the thermally conductive resin 6 if it has improved thermal conductivity, a thermally conductive flexible resin whose shape can be changed according to the outer shape and outer diameter of the column 7 to be accommodated is preferable. By using this sort of resin, temperature can be accurately controlled in contact with the column 7 without any gap regardless of the outer shape or the like of the column 7.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は液体クロマトグラフ
装置に用いられるカラム恒温装置に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a column thermostat used in a liquid chromatograph.

【0002】[0002]

【従来の技術】カラム恒温装置として、カラムに装着し
恒温水を流すジャケット装置、カラムを丸ごと浸す恒温
水装置、アルミ等の金属ブロックにカラムを挟むブロッ
ク恒温装置、筐体内部の空気温度を一定に保つとともに
該内部にカラムを収納する空気恒温装置が知られてい
る。
2. Description of the Related Art As a column constant temperature device, a jacket device mounted on a column and flowing constant temperature water, a constant temperature water device for immersing the entire column, a block constant temperature device for sandwiching the column between metal blocks of aluminum or the like, and a constant air temperature inside the housing. There is known an air thermostat in which a column is kept inside and a column is housed therein.

【0003】[0003]

【発明が解決しようとする課題】カラムに装着し恒温水
を流すジャケット装置やカラムを丸ごと浸す恒温水装置
は、実験用途で頻繁に用いられる。しかし、これら恒温
装置では熱媒体として使用する水が汚濁等し易く、定期
的にメンテナンスを行ってこれを交換しなければならな
いという使用上の課題がある。
A jacket device which is attached to a column and in which constant temperature water flows and a constant temperature water device in which the entire column is immersed are frequently used for experimental purposes. However, in these constant temperature apparatuses, water used as a heat medium is liable to be polluted or the like, and there is a problem in use in that maintenance must be periodically performed and replaced.

【0004】アルミ等の金属ブロックにカラムを挟むブ
ロック恒温装置は液体を使用しないため前記のような課
題は生じないが、カラムと金属ブロックの間に隙間があ
ると熱伝導の効率が低下する。従って、多種多様の外形
・外径を有するカラムを使用する場合はカラム毎の熱伝
導効率の変動を考慮するか、又はカラム外形・外径に対
応するブロックに換装して使用しなければならないとい
う課題がある。しかも、カラム形状は単なる円柱状では
なく、特にその両端のエンドフィティング部は他の部分
とは異なる外形・外径を有していることがあるため、か
かるカラムに適合した金属ブロックを製造すること自体
が困難であるという問題がある。また更には、カラムを
交換する場合には金属ブロックをはずさなければならな
い等、メンテナンス上の課題もある。
[0004] The above-mentioned problem does not occur in a block thermostat in which a column is sandwiched between metal blocks of aluminum or the like because no liquid is used. However, if there is a gap between the column and the metal block, the efficiency of heat conduction is reduced. Therefore, when using columns having a wide variety of outer shapes and outer diameters, it is necessary to consider the fluctuations in the heat transfer efficiency of each column, or to replace and use blocks corresponding to the outer shapes and outer diameters of the columns. There are issues. In addition, the column shape is not merely a columnar shape, and in particular, since the end fitting portions at both ends may have different outer shapes and outer diameters from other portions, a metal block suitable for such a column is manufactured. There is a problem that it is difficult. In addition, there is a problem in maintenance such as the need to remove the metal block when replacing the column.

【0005】ブロック恒温装置の場合、カラムと金属ブ
ロックの間に熱伝導性グリースを塗って熱伝導性を改善
する等の手法により、ある程度は外形や外径の異なるカ
ラムに対応することも可能であるが、この場合にはグリ
ースによりカラムが汚染されるという新たな課題が生じ
る。
[0005] In the case of a block thermostat, it is possible to cope with columns having different external shapes and outer diameters to some extent by a method such as applying a thermal conductive grease between the column and the metal block to improve the thermal conductivity. However, in this case, there is a new problem that the column is contaminated with grease.

【0006】筐体内部の空気温度を一定に保つとともに
該内部にカラムを収納する空気恒温装置は、カラムの外
形・外径等の寸法形状に関係なく使用でき、しかもカラ
ムの脱着等のメンテナンスも容易であるが、空気は体積
あたりの熱容量が小さいため正確な温度制御は困難であ
るという課題がある。
An air thermostat that keeps the air temperature inside the housing constant and houses the column inside the housing can be used irrespective of the dimensions and shape of the column, such as the outer diameter and outer diameter, and also allows maintenance such as desorption of the column. Although easy, air has a problem that accurate temperature control is difficult due to small heat capacity per volume.

【0007】そこで本発明の目的は、上記した従来のカ
ラム恒温装置における課題を解決し、カラムの脱着等の
メンテナンスを容易に行い得、しかもグリス等を用いて
カラムを汚染することなしに多種多様の外形・外径を有
するカラムについて正確な温度制御を可能とするカラム
恒温装置を提供することにある。
Accordingly, an object of the present invention is to solve the above-mentioned problems of the conventional column thermostat, to easily perform maintenance such as desorption of the column, and to perform various operations without contaminating the column with grease or the like. It is an object of the present invention to provide a column thermostat capable of accurately controlling the temperature of a column having an outer diameter and an outer diameter.

【0008】[0008]

【課題を解決するための手段】上記目的を達成するため
に成された本発明のカラム恒温装置は、内部にカラムを
収納する熱伝導体で形成された筐体と筐体に熱的に連絡
された温度制御手段とから構成されるカラム恒温装置に
おいて、内部に収納されるカラムの少なくとも一部と筐
体とを熱的に連絡する熱伝導性樹脂を装備したことを特
徴とするカラム恒温装置である。以下、本発明のカラム
恒温装置を図面に示した実施の形態に基づき詳細に説明
する。
Means for Solving the Problems To achieve the above object, a column thermostat of the present invention is provided. A column formed of a heat conductor accommodating a column therein is thermally connected to the column. Column thermostat comprising a temperature control means provided with a thermally conductive resin for thermally communicating at least a part of the column housed therein and the housing. It is. Hereinafter, a column thermostat of the present invention will be described in detail based on an embodiment shown in the drawings.

【0009】[0009]

【発明の実施の形態】図1は本発明のカラム恒温装置の
外観を、図2はその断面図を示すものである。カラム恒
温装置の筐体1は、熱伝導体であるアルミニウム等の金
属で構成する。筐体の外面には発泡ウレタンゴム等の断
熱材2を貼ることが好ましい。また断熱材を金属製の箱
等で覆うことが特に好ましい。
FIG. 1 shows the appearance of a column thermostat of the present invention, and FIG. 2 shows a sectional view thereof. The housing 1 of the column thermostat is made of a metal such as aluminum which is a heat conductor. It is preferable to attach a heat insulating material 2 such as urethane foam rubber to the outer surface of the housing. It is particularly preferable to cover the heat insulating material with a metal box or the like.

【0010】筐体は、その内部空間3が多種多様の外形
・外径を有するカラムを収納するのに充分となるように
構成する。例えば図1又は2のカラム恒温装置は、直径
4.7mm、長さ10cmのカラム(両端のエンドフィ
ッティングを含め、全長約15cm)の分析用カラム
(図中央)及び前処理用カラムの両者を収納し得る大き
さに構成した。なお図1又は2の例では、恒温装置に機
械的強度を付与するため、発泡ウレタンゴムの外側を更
に鋼板で覆ってある。
The housing is constructed so that its internal space 3 is sufficient to accommodate columns having a wide variety of external and external diameters. For example, the column thermostat of FIG. 1 or 2 accommodates both a 4.7 mm diameter column and a 10 cm length column (approximately 15 cm in length including end fittings at both ends) for analysis (center of the figure) and for pretreatment. The size was set to be as large as possible. In the example of FIG. 1 or 2, the outside of the urethane foam rubber is further covered with a steel plate in order to impart mechanical strength to the thermostat.

【0011】筐体は、内側にカラム7を設置し、更には
収納されたカラムを交換する等のメンテナンスを容易に
するため、少なくとも2の部品、例えば本体Aと蓋Bに
分割される。また好ましくは本体の一面にヒータ又は熱
電子素子等の発熱源(冷却源)4を熱的に連絡した状態
で配置するが、筐体内部に配置することも可能である。
また温度制御のため、好ましくは本体に例えば白金温度
センサ等の温度センサ5を取り付け、温度センサ、発熱
源(冷却源)と温度センサで検知された筐体温度又は筐
体内部温度に基づき、発熱源(冷却源)を操作して筐体
を加温又は冷却し、予め設定された温度に制御する不図
示のマイクロコンピュータ等により制御手段を構成す
る。本発明でいう熱的な連絡とは、連絡される手段又は
部材間で熱が伝達されるような関係を意味し、その程度
は問わない。
The housing is divided into at least two parts, for example, a main body A and a lid B, in order to facilitate maintenance such as installing the column 7 inside and further replacing the stored column. Preferably, a heat source (cooling source) 4 such as a heater or a thermoelectric element is arranged on one surface of the main body in a state of being in thermal communication with the heat source, but it may be arranged inside the housing.
For temperature control, preferably, a temperature sensor 5 such as a platinum temperature sensor is attached to the main body, and heat is generated based on the temperature sensor, a heat source (cooling source), and a housing temperature or a housing internal temperature detected by the temperature sensor. A control unit is constituted by a microcomputer (not shown) or the like that operates a source (cooling source) to heat or cool the housing, and controls the temperature to a preset temperature. The term "thermal communication" as used in the present invention means a relation in which heat is transmitted between means or members to be communicated, and the degree is not limited.

【0012】本発明で使用する熱伝導性樹脂6として
は、熱伝導が良好であれば制限はないが、収納するカラ
ムの外形・外径に応じて形状を変化し得る熱伝導性可撓
性樹脂が特に好ましい。かかる樹脂を使用することによ
り、カラムの外形等にかかわらずこれと隙間なく接触し
てカラム温度を正確に制御し得るという効果が達成され
る。
The heat conductive resin 6 used in the present invention is not limited as long as it has good heat conductivity, but the heat conductive resin 6 can change its shape according to the outer shape and outer diameter of the column to be stored. Resins are particularly preferred. By using such a resin, it is possible to achieve an effect that the column temperature can be accurately controlled by contacting the resin without any gap irrespective of the outer shape of the column.

【0013】熱伝導性可曉性樹脂としては、例えば放熱
シリコーンゴムシート等、半導体の放熱に用いられてい
るものが使用できる。一例として市販の樹脂(サーコン
(登録商標)GR、富士高分子工業(株)製)を例示で
きる。これら樹脂の熱伝導率は約2W ・m−1・K −1
程度で、アルミニウムの1/100倍、ステンレスの1
/10倍であるが、通常のプラスチックの10倍であ
る。本発明ではこれら例示した樹脂以外の、例えばより
高い熱伝導率を有する樹脂を用いることに制限はない。
熱伝導性可撓性樹脂の可撓性、即ち柔軟性は高いほど好
ましい。カラムを樹脂に押し付けた時に容易にへこむ程
度の可撓性を有していることが特に好ましい。
As the heat conductive resin, a resin used for heat radiation of a semiconductor such as a heat radiation silicone rubber sheet can be used. As an example, a commercially available resin (Sircon (registered trademark) GR, manufactured by Fuji Polymer Co., Ltd.) can be exemplified. The thermal conductivity of these resins is about 2W · m-1 · K -1
1/100 times of aluminum, 1 of stainless steel
/ 10 times that of ordinary plastics. In the present invention, there is no limitation to use a resin having a higher thermal conductivity, for example, other than these exemplified resins.
The higher the flexibility of the heat conductive flexible resin, that is, the higher the flexibility, the better. It is particularly preferable that the column has such flexibility that the column is easily dented when pressed against the resin.

【0014】本発明のカラム恒温装置は、前記した熱伝
導性可撓性樹脂により内部に収納されるカラムの少なく
とも一部が筐体と熱的に連絡され得るものである。より
具体的には、筐体の内面に樹脂を一重以上に敷き詰め、
カラムを該樹脂に接触した状態で収納し得るように構成
された装置を例示できる。本発明において好ましくは、
カラム全面を熱伝導性可撓樹脂で包み込み、又は、図2
に示したように1対(2枚)の熱伝導性可撓性樹脂を使
用してこれらで収納したカラムを挟み込むようにするこ
とである。かかる構成では、図中カラムの上面及び下面
が樹脂と接触し、下面の樹脂は筐体と連絡しているた
め、温度制御を更に容易かつ正確に行い得る。特に後者
の構成では、カラムを脱着する場合でも上側の樹脂を取
りはずすのみで足りるからである。
In the column thermostat of the present invention, at least a part of the column housed inside by the heat conductive flexible resin can be in thermal communication with the housing. More specifically, the resin is spread more than once on the inner surface of the housing,
An example of a device configured to be able to store a column in contact with the resin can be given. In the present invention, preferably,
Wrap the entire column with a thermally conductive flexible resin, or
As shown in (1), a pair of (two) thermally conductive flexible resins is used to sandwich a column housed between them. In such a configuration, the upper surface and the lower surface of the column in the figure are in contact with the resin, and the resin on the lower surface is in communication with the housing, so that the temperature control can be performed more easily and accurately. In particular, in the latter configuration, it is sufficient to remove only the upper resin even when the column is detached.

【0015】図2に示したように2枚の樹脂を用いる場
合、その一方が筐体に熱的に連絡していれば十分である
が、両者が熱的に熱的に筐体と連絡していることが特に
好ましい。また、カラムとの連絡は、その長手方向全般
に渡っていることが特に好ましい。このように熱伝導性
可撓性樹脂はできるだけ広い範囲に渡って筐体と連絡し
ていることが好ましい。
When two resins are used as shown in FIG. 2, it is sufficient if one of them is in thermal communication with the housing, but both are in thermal communication with the housing. Is particularly preferred. It is particularly preferred that the communication with the column extends over the entire length thereof. As described above, it is preferable that the heat conductive flexible resin is in communication with the housing over as wide a range as possible.

【0016】熱伝導性可撓樹脂が熱的に連絡する筐体部
分に特別の制限はないが、前記したようにカラム恒温装
置において本体と蓋部を設ける場合では、可動性である
蓋部との接触よりも不動部である本体と連絡させること
が好ましい。蓋部及び本体の両方と熱的に連絡させる場
合には、蓋部を閉じることにより両部と熱伝導性可撓樹
脂及びカラムが互いに圧着されるようにすることが特に
好ましい。
Although there is no particular limitation on the case portion to which the heat conductive flexible resin is in thermal communication, as described above, when the main body and the cover are provided in the column thermostat, the movable cover and the cover may be used. It is preferable to contact the main body, which is an immovable part, rather than the contact of the main body. When thermally communicating with both the lid and the main body, it is particularly preferable that the lid, the thermally conductive flexible resin, and the column be pressed against each other by closing the lid.

【0017】カラム恒温装置内に収納されたカラムは、
分析されるべき試料液を送液するための配管により外部
のポンプ等と連結されているが、配管を通ってカラムに
供される液体はカラム恒温装置内部の温度と異なるのが
普通である。このように温度の異なる液体がカラム内に
導入されると、カラム内部温度を制御することが困難に
なる。そこで本発明のカラム恒温装置では、好ましくは
カラム入口側の配管の少なくとも一部を前記熱伝導性樹
脂と熱的に連絡させる。熱伝導性樹脂と熱的に連絡させ
る配管部分は、通常の送液速度で送液された液体が配管
を通過してカラムに導入される過程でカラム温度と同程
度に加温又は冷却されるのに充分であることが好まし
い。かかる目的を達成するためには、図2に示したよう
に2枚の樹脂を使用し、その間に配管8を挟み込む構成
を例示できる。なお図2の構成では、熱伝導性可撓性樹
脂を合計3枚使用した例である。
The column housed in the column thermostat is:
Although connected to an external pump or the like by a pipe for sending the sample liquid to be analyzed, the liquid supplied to the column through the pipe is usually different from the temperature inside the column thermostat. When the liquids having different temperatures are introduced into the column, it becomes difficult to control the temperature inside the column. Therefore, in the column thermostat of the present invention, preferably, at least a part of the pipe on the column inlet side is in thermal communication with the heat conductive resin. The pipe portion that is in thermal communication with the heat conductive resin is heated or cooled to the same temperature as the column temperature in the process in which the liquid sent at a normal liquid sending speed passes through the pipe and is introduced into the column. Is preferably sufficient. In order to achieve this object, a configuration in which two resins are used as shown in FIG. 2 and the pipe 8 is interposed therebetween can be exemplified. The configuration in FIG. 2 is an example in which a total of three thermally conductive flexible resins are used.

【0018】[0018]

【発明の効果】本発明のカラム恒温装置によれば、多種
多様の外形・外径を有するカラム、言い換えれば異なる
直径、長さのカラムを収納し、高い精度と正確性でカラ
ム温度を制御し得るカラム恒温装置が提供される。また
更には、カラムが熱伝導性可撓性樹脂によって間接的に
筐体に接触しているため、筐体温度の細かな変動の影響
を受け難いという効果も達成されることになる。
According to the column thermostat of the present invention, columns having various external shapes and outer diameters, in other words, columns having different diameters and lengths are accommodated, and the column temperature is controlled with high precision and accuracy. A resulting column thermostat is provided. Furthermore, since the column is indirectly in contact with the housing by the heat conductive flexible resin, an effect of being hardly affected by a small fluctuation of the housing temperature can be achieved.

【図面の簡単な説明】[Brief description of the drawings]

【図1】図1はカラム恒温装置の外観図である。FIG. 1 is an external view of a column thermostat.

【図2】図2はカラム恒温装置の断面図である。FIG. 2 is a sectional view of a column thermostat.

【符号の説明】[Explanation of symbols]

1 筐体、2 断熱材、3 内部空間、4 発熱源(冷
却源)、5 温度センサ、6 熱伝導性可撓性樹脂、7
カラム、8 配管、A 本体、B 蓋部
Reference Signs List 1 housing, 2 heat insulating material, 3 internal space, 4 heat source (cooling source), 5 temperature sensor, 6 heat conductive flexible resin, 7
Column, 8 piping, A body, B lid

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】内部にカラムを収納する熱伝導体で形成さ
れた筐体と筐体に熱的に連絡された温度制御手段とから
構成されるカラム恒温装置において、内部に収納される
カラムの少なくとも一部と筐体とを熱的に連絡する熱伝
導性樹脂を装備したことを特徴とするカラム恒温装置。
1. A column thermostat comprising a housing formed of a heat conductor accommodating a column therein and temperature control means thermally connected to the housing. A column thermostat comprising a thermally conductive resin for thermally communicating at least a part of the column with a housing.
【請求項2】熱伝導性樹脂が、内部に収容されるカラム
の全面を覆うように配置されていることを特徴とする請
求項1の装置。
2. The apparatus according to claim 1, wherein the heat conductive resin is disposed so as to cover the entire surface of the column accommodated therein.
【請求項3】更に、前記熱伝導性樹脂がカラムの入口側
配管の少なくとも一部と熱的に連絡することを特徴とす
る請求項1の装置。
3. The apparatus of claim 1 wherein said thermally conductive resin is in thermal communication with at least a portion of the column inlet piping.
JP20475798A 1998-07-21 1998-07-21 Column thermostat Expired - Fee Related JP3982071B2 (en)

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