JP2005265807A - Sample cooler unit - Google Patents

Sample cooler unit Download PDF

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Publication number
JP2005265807A
JP2005265807A JP2004083020A JP2004083020A JP2005265807A JP 2005265807 A JP2005265807 A JP 2005265807A JP 2004083020 A JP2004083020 A JP 2004083020A JP 2004083020 A JP2004083020 A JP 2004083020A JP 2005265807 A JP2005265807 A JP 2005265807A
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Prior art keywords
sample
sample container
rack
support member
cooled
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Japanese (ja)
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Kenichi Yasunaga
研壱 保永
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Shimadzu Corp
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Shimadzu Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample cooler unit hardly generating temperature unevenness in a sample container. <P>SOLUTION: A rack 1 cooled via a metal block 23 by a cooler (Peltier element 21) is constituted of a heat transferring casing 3, an upper support member 7 and a bottom part support member 8, and the sample container 2 stored in an inside thereof is supported by the two support members not to contact directly with the heat transferring casing 3. The cooling is moderate since the sample container 2 is cooled substantially via air, by this constitution, and the temperature unevenness is hardly generated because quick cooling is not occurred locally. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は液体試料を自動的に分析する分析装置、特に液体クロマトグラフにおいて分析前の試料を冷却する試料冷却装置に関する。   The present invention relates to an analyzer that automatically analyzes a liquid sample, and more particularly to a sample cooling device that cools a sample before analysis in a liquid chromatograph.

液体クロマトグラフにおける自動分析は、予め少量の試料を封入した試料容器をラックに装架し、このラックを自動試料注入装置にセットし、自動試料注入装置がこのラック上の試料容器から所定プログラムに従って逐次に試料を吸い上げ、液体クロマトグラフに注入することにより実行される。分析待ち状態にあるラック上の試料は多くの場合は室温下に置かれるが、試料によっては、変質を防ぐために低温に保つことが必要な場合がある。このような場合に、試料を冷却する目的に使われる装置が試料冷却装置である。   In automatic analysis in a liquid chromatograph, a sample container filled with a small amount of sample in advance is mounted on a rack, this rack is set in an automatic sample injection device, and the automatic sample injection device starts from the sample container on this rack according to a predetermined program. This is performed by sequentially sucking up the sample and injecting it into the liquid chromatograph. Samples on the rack that are waiting for analysis are often placed at room temperature, but some samples may need to be kept at a low temperature to prevent alteration. In such a case, an apparatus used for the purpose of cooling the sample is a sample cooling apparatus.

図2は従来の試料冷却装置の一例を自動試料注入装置内にセットされた状態で示したものである。
分析者は、まず液体試料4を試料容器2(通常はガラス製の小瓶)に入れ、ラック5に装架する。ラック5は伝熱性に優れたアルミ製で、試料容器2を挿入する100個程の穴5aが穿設されている。この穴5aの底および内壁を通して試料容器2に熱(以下、単に熱と記す場合は冷熱を含むものとする)が伝えられる。
FIG. 2 shows an example of a conventional sample cooling apparatus set in an automatic sample injection apparatus.
The analyst first places the liquid sample 4 in the sample container 2 (usually a glass vial) and mounts it on the rack 5. The rack 5 is made of aluminum having excellent heat conductivity, and has about 100 holes 5a into which the sample containers 2 are inserted. Heat is transmitted to the sample container 2 through the bottom and the inner wall of the hole 5a (hereinafter, simply referred to as heat includes cold heat).

液体試料4を装填し終わったラック5は装置内の金属ブロック23の上に載置される。金属ブロック23は、下面に取り付けた冷却器(ペルチエ素子21)によって冷却され、上面がラック5の底に密着して良好な熱伝導を保つ。
ペルチエ素子21は、図示しない温度調節装置によってコントロールされてその吸熱面で金属ブロック23を所定温度に冷却し、その裏面(放熱面)には、通風ダクト27の内側に面して放熱フィン22が取り付けられ、金属ブロック23から吸収した熱をこの放熱フィン22を通してファン28による送風で放熱する構造となっている。
このような構成で、ラック5とこれに装架された試料容器2、さらにはその中の液体試料4が所定の低温に保たれる。ラック5は保冷のため断熱性のカバー6で覆われるが、試料容器2の頭部は、ニードル11による液体試料4の取り出しを可能にするため、このカバー6から露出し、室温の空気に曝されている。
The rack 5 loaded with the liquid sample 4 is placed on the metal block 23 in the apparatus. The metal block 23 is cooled by a cooler (Peltier element 21) attached to the lower surface, and the upper surface is in close contact with the bottom of the rack 5 to maintain good heat conduction.
The Peltier element 21 is controlled by a temperature control device (not shown) to cool the metal block 23 to a predetermined temperature on its heat absorption surface, and on its back surface (heat radiation surface), the heat radiation fins 22 face the inside of the ventilation duct 27. It is attached and has a structure in which the heat absorbed from the metal block 23 is radiated by the air blown by the fan 28 through the radiating fins 22.
With such a configuration, the rack 5, the sample container 2 mounted on the rack 5, and the liquid sample 4 therein are kept at a predetermined low temperature. The rack 5 is covered with a heat-insulating cover 6 for cold insulation, but the head of the sample container 2 is exposed from the cover 6 and exposed to room temperature air so that the liquid sample 4 can be taken out by the needle 11. Has been.

自動試料注入装置10のニードル11は、図示しないメカニズムにより前後左右および上下に移動可能で、プログラムに従って、試料容器2から液体試料4を吸い上げ、液体クロマトグラフの試料注入口12まで移動してこれに液体試料4を注入することによって自動分析が行われる。液体クロマトグラフの分析は1回数十分を要するので、ラック5上の液体試料4は長いもので数十時間も分析待ち状態となるが、この間、低温に保たれることで液体試料4の変質が避けられる。   The needle 11 of the automatic sample injection device 10 can be moved back and forth, right and left and up and down by a mechanism (not shown). According to the program, the needle 11 sucks the liquid sample 4 and moves to the sample inlet 12 of the liquid chromatograph. Automatic analysis is performed by injecting a liquid sample 4. Since the liquid chromatograph needs to be analyzed once enough, the liquid sample 4 on the rack 5 is long and is waiting for analysis for several tens of hours. During this time, the liquid sample 4 is kept at a low temperature to avoid alteration of the liquid sample 4. It is done.

上記のように構成された試料冷却装置においては、試料容器2は主に底の方から冷却されるので内部の液体試料4に温度ムラを生じることがあり、これを解消するために、試料容器2の底とラック5との間に断熱性部材を介在させて、試料容器2の底部からの伝熱を抑制するようにした例もある(例えば、特許文献1参照)。   In the sample cooling apparatus configured as described above, since the sample container 2 is mainly cooled from the bottom, temperature irregularity may occur in the internal liquid sample 4, and in order to eliminate this, the sample container There is also an example in which a heat insulating member is interposed between the bottom of 2 and the rack 5 to suppress heat transfer from the bottom of the sample container 2 (see, for example, Patent Document 1).

特開2000−137031号公報JP 2000-137031 A

前述のように、試料容器2の頭部は室温の空気中に露出していること、及び、構造上ラック5は主として下から冷却されることから、試料容器2は底が冷たく上部は温かいという状態、つまり温度ムラが生じ勝ちである。しかも、下方が低温となるために対流が起こらないので、温度ムラは時間が経過しても解消せず、持続する傾向にある。試料容器2に温度ムラがあると、その内部の液体試料4に濃度ムラが生じる場合があり、そのような状態でサンプリングすると分析結果にバラツキが生じることがある。   As described above, since the head of the sample container 2 is exposed to air at room temperature, and the rack 5 is structurally cooled mainly from below, the sample container 2 is said to have a cold bottom and a warm upper part. State, that is, temperature unevenness is likely to occur. In addition, since convection does not occur because the lower temperature is low, the temperature unevenness does not disappear even when time passes and tends to persist. If the sample container 2 has temperature unevenness, the liquid sample 4 in the sample container 2 may have concentration unevenness. If sampling is performed in such a state, the analysis result may vary.

特許文献1に記されたように、試料容器の底部からの伝熱を抑制する構造にすれば、この問題解消に一定の効果はあるが、なお万全とは言い難いのが現状である。
本発明は、このような事情に鑑みてなされたものであり、上記のような温度ムラの生じにくい試料冷却装置を提供することを目的とする。
As described in Patent Document 1, if a structure that suppresses heat transfer from the bottom of the sample container is used, there is a certain effect in solving this problem, but it is still difficult to say that it is perfect.
The present invention has been made in view of such circumstances, and an object of the present invention is to provide a sample cooling apparatus that hardly causes temperature unevenness as described above.

本発明は、上記課題を解決するために、冷却された伝熱性筐体内に試料容器を収め、その試料容器が伝熱性筐体に直接接触しないように支持する構造とした。即ち、本発明装置は、底部から冷却器によって冷却される伝熱性筐体内に試料容器を配列して収納するように構成されたラックを備える試料冷却装置において、前記試料容器が前記伝熱性筐体の内面に接触することなく前記試料容器を所定位置に支持する支持部材を備えたことを特徴とする試料冷却装置である。
このように構成したことにより、試料容器が局所的に冷却されることによる液体試料の温度ムラが解消される。
In order to solve the above-mentioned problems, the present invention has a structure in which a sample container is housed in a cooled heat conductive casing and is supported so that the sample container does not directly contact the heat conductive casing. That is, the apparatus of the present invention is a sample cooling apparatus including a rack configured to arrange and store sample containers in a heat conductive casing cooled by a cooler from the bottom, wherein the sample container is the heat conductive casing. A sample cooling apparatus comprising a support member that supports the sample container at a predetermined position without contacting the inner surface of the sample container.
With this configuration, the temperature unevenness of the liquid sample due to the local cooling of the sample container is eliminated.

本発明装置は、上記のように、試料容器を伝熱性筐体に直接接触しないように支持して主に空気を介して冷却するように構成されているので、試料容器は底部が強く冷却されることがなく、その内部の試料液体に温度ムラが発生しにくい。その結果、温度差に基づく濃度ムラも抑制されるので、分析の再現性が向上する。   As described above, the apparatus of the present invention is configured to support the sample container so that it does not directly contact the heat-conducting housing and to cool mainly through air, so that the bottom of the sample container is strongly cooled. And temperature unevenness hardly occurs in the sample liquid inside. As a result, density unevenness based on the temperature difference is also suppressed, so that the reproducibility of the analysis is improved.

本発明の一実施形態を図1に示す。同図において、図2と同一の構成要素には同一符号を付してあるので再度の説明を省く。
本実施形態が従来と異なる点はラック1の構造にある。即ち、ラック1は、上部が開いた箱形の伝熱性筐体3と、その上部を掩覆する上部支持部材7、及びラック1の内部底面に置かれた底部支持部材8とで構成される。
One embodiment of the present invention is shown in FIG. In the figure, the same components as those in FIG.
This embodiment is different from the conventional one in the structure of the rack 1. That is, the rack 1 includes a box-shaped heat conductive housing 3 having an open top, an upper support member 7 that covers the upper portion, and a bottom support member 8 that is placed on the inner bottom surface of the rack 1. .

伝熱性筐体3は、金属ブロック23の上に密接して載置され、金属ブロック23からの伝熱により底の方から冷却され、これに触れる内部の空気が冷却される。
上部支持部材7は、硬質プラスチック等で製作され、試料容器2を挿入するための多数の穴7aが所定位置に配列されており、これに挿入された試料容器2の水平方向の位置を規制する。穴7aは、最も端に位置するものでもそこに挿入される試料容器2が伝熱性筐体3の壁面に接触しないように配置される。
底部支持部材8は、試料容器2を下から支持して、試料容器2の底が伝熱性筐体3の底に接触することを防ぐもので、硬質プラスチックまたは伝熱性のあまり良くない金属(例えば、ステンレス鋼)の薄板で製作される。
The heat transfer housing 3 is placed in close contact with the metal block 23, cooled from the bottom by heat transfer from the metal block 23, and the internal air that touches this is cooled.
The upper support member 7 is made of hard plastic or the like, and a large number of holes 7a for inserting the sample container 2 are arranged at predetermined positions, and the horizontal position of the sample container 2 inserted therein is regulated. . Even if the hole 7a is located at the end, the sample container 2 inserted therein is arranged so as not to contact the wall surface of the heat conductive casing 3.
The bottom support member 8 supports the sample container 2 from below and prevents the bottom of the sample container 2 from coming into contact with the bottom of the heat transfer casing 3. The bottom support member 8 is made of hard plastic or a metal with poor heat transfer (for example, , Stainless steel).

このように構成された本実施形態による試料の冷却は以下のように行われる。
ペルチエ素子21により冷却された金属ブロック23からの伝熱により、まず伝熱性筐体3が冷却され、これにより冷却された空気を介して試料容器2、さらにはその内部の液体試料4が冷却される。試料容器2は、いずれも伝熱性の良くない上部支持部材7と底部支持部材8によって伝熱性筐体3に直接接触しないように支持されているので、ほぼ完全に空気のみを介して冷却されることになる。従って、冷却は緩やかであり、局所的に急速な冷却が起こることはないので温度ムラも生じにくい。
The cooling of the sample according to the present embodiment configured as described above is performed as follows.
The heat transfer case 3 is first cooled by heat transfer from the metal block 23 cooled by the Peltier element 21, and the sample container 2 and further the liquid sample 4 inside thereof are cooled through the air thus cooled. The The sample container 2 is supported by the upper support member 7 and the bottom support member 8 which are not good in heat transfer so as not to come into direct contact with the heat transfer case 3, and thus is almost completely cooled only by air. It will be. Therefore, the cooling is slow and rapid local cooling does not occur, so that temperature unevenness hardly occurs.

底部支持部材8は、これを挟む上下の空間を空気が流通する必要があるので、通気性のあるパンチングメタルや金網等を用いて構成してもよい。また、図1に示すような底から立ち上げる構造に限らず、底に接して敷設する構造や適当なスペーサ(図示しない)を介して上部支持部材7から吊設する構造も可能である。   Since the bottom support member 8 needs to circulate air in the upper and lower spaces sandwiching the bottom support member 8, it may be configured by using a punching metal or a wire net having air permeability. In addition to the structure rising from the bottom as shown in FIG. 1, a structure laid in contact with the bottom or a structure suspended from the upper support member 7 through an appropriate spacer (not shown) is also possible.

上部支持部材7は冷気をラック1の内部に閉じ込める役割も負っているので、断熱性素材を用いて構成し、必要に応じ、さらに断熱性カバー(図示しない)をその上に被せて保冷効果を高めるようにしてもよい。また、保冷効果を高める別の手段として、試料容器2が挿入されていない穴7aは断熱性の栓(図示しない)で塞ぐようにしてもよい。   Since the upper support member 7 also has a role of confining cold air inside the rack 1, the upper support member 7 is made of a heat insulating material, and if necessary, a heat insulating cover (not shown) is put on the heat insulating material to provide a cooling effect. You may make it raise. Further, as another means for enhancing the cooling effect, the hole 7a in which the sample container 2 is not inserted may be closed with a heat insulating plug (not shown).

下から冷却される本実施形態では、対流が起こりにくく、冷気がラック1の底近くに停滞することが危惧される。この対策として、図示しない送風装置でラック1の内部空気を攪拌し、温度の均一化を図ることは設計事項として容易に考えられる。
なお、上記は本発明の基本的構成といくつかの変形例を示したものであって、本発明をこれに限定するものではない。
In the present embodiment, which is cooled from below, convection is unlikely to occur, and there is a concern that the cold air is stagnating near the bottom of the rack 1. As a countermeasure, it is easily considered as a design matter to stir the internal air of the rack 1 with a blower (not shown) to make the temperature uniform.
The above shows the basic configuration of the present invention and some modifications, and the present invention is not limited to this.

本発明の一実施形態を示す図である。It is a figure which shows one Embodiment of this invention. 従来の構成を示す図である。It is a figure which shows the conventional structure.

符号の説明Explanation of symbols

1 ラック
2 試料容器
3 伝熱性筐体
4 液体試料
5 ラック
5a 穴
6 カバー
7 上部支持部材
7a 穴
8 底部支持部材
10 自動試料注入装置
11 ニードル
12 試料注入口
21 ペルチエ素子
22 放熱フィン
23 金属ブロック
27 通風ダクト
28 ファン
DESCRIPTION OF SYMBOLS 1 Rack 2 Sample container 3 Heat conductive housing 4 Liquid sample 5 Rack 5a Hole 6 Cover 7 Upper support member 7a Hole 8 Bottom support member 10 Automatic sample injection device 11 Needle 12 Sample injection port 21 Peltier element 22 Radiation fin 23 Metal block 27 Ventilation duct 28 Fan

Claims (1)

ラックに装架された試料容器内の液体試料を室温以下に冷却する試料冷却装置であって、前記ラックは底部から冷却器によって冷却される伝熱性筐体内に前記試料容器を配列して収納するように構成されたものにおいて、前記試料容器が前記伝熱性筐体の内面に接触することなく前記試料容器を所定位置に支持する支持部材を備えたことを特徴とする試料冷却装置。 A sample cooling apparatus for cooling a liquid sample in a sample container mounted on a rack to room temperature or lower, wherein the rack arranges and stores the sample containers in a heat conductive casing cooled by a cooler from the bottom. What is comprised in this way, The sample cooling device provided with the supporting member which supports the said sample container in a predetermined position, without contacting the said sample container with the inner surface of the said heat conductive housing | casing.
JP2004083020A 2004-03-22 2004-03-22 Sample cooler unit Pending JP2005265807A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009264815A (en) * 2008-04-23 2009-11-12 Nikkiso Co Ltd Osmotic pressure analyzer
WO2015162680A1 (en) * 2014-04-22 2015-10-29 株式会社島津製作所 Sample rack for heating temperature adjustment and sample temperature adjustment device using said sample rack for heating temperature adjustment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009264815A (en) * 2008-04-23 2009-11-12 Nikkiso Co Ltd Osmotic pressure analyzer
WO2015162680A1 (en) * 2014-04-22 2015-10-29 株式会社島津製作所 Sample rack for heating temperature adjustment and sample temperature adjustment device using said sample rack for heating temperature adjustment

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