JP4492466B2 - Sample thermostat - Google Patents

Sample thermostat Download PDF

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JP4492466B2
JP4492466B2 JP2005201977A JP2005201977A JP4492466B2 JP 4492466 B2 JP4492466 B2 JP 4492466B2 JP 2005201977 A JP2005201977 A JP 2005201977A JP 2005201977 A JP2005201977 A JP 2005201977A JP 4492466 B2 JP4492466 B2 JP 4492466B2
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sample container
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recess
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JP2007017403A (en
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隆志 井上
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Shimadzu Corp
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Description

本発明は液体クロマトグラフや生化学自動分析装置などの分析の分野において試料を均一且つ一定温度に保つための装置に関する。   The present invention relates to an apparatus for maintaining a sample at a uniform and constant temperature in the field of analysis such as a liquid chromatograph and a biochemical automatic analyzer.

液体クロマトグラフなどでは、多数の試料を次々と自動的に分析できるようになっている。それらの試料は、上方から挿入される吸込用針により採取が可能なように、中央付近に切り込みがあるゴム製の栓で詰められた開口部が設けられた蓋が付いた試料容器に充填されており、その試料容器は、測定値の再現性や測定精度の向上のために、均一且つ一定の温度に保たれる。そのために、試料容器は、複数個の凹部を設けた恒温ブロックに装填されており、その恒温ブロックを一定温度に制御することにより試料温度を一定に保っている。恒温ブロックは銅や真鍮などの熱伝導の良い材料で構成されており、恒温ブロックの凹部は、試料容器の外形に応じた形に形成され、試料容器と密に接触することによって熱伝導が良好に保たれているため、試料容器の温度は恒温ブロックとほぼ同温に保たれる。恒温ブロックにはペルチェ素子等の加熱冷却素子が組み込まれた温調部が密着しており、素子に与える電圧を制御することによって、恒温ブロックの温度を制御している（例えば、特許文献１参照）。   In a liquid chromatograph or the like, a large number of samples can be automatically analyzed one after another. These samples are filled in a sample container with a lid provided with an opening filled with a rubber stopper with a notch near the center so that it can be collected by a suction needle inserted from above. The sample container is kept at a uniform and constant temperature in order to improve the reproducibility of measurement values and the measurement accuracy. Therefore, the sample container is loaded in a constant temperature block provided with a plurality of recesses, and the temperature of the sample is kept constant by controlling the constant temperature block to a constant temperature. The thermostatic block is made of a material with good thermal conductivity such as copper or brass, and the recess of the thermostatic block is formed in a shape according to the outer shape of the sample container, and the heat conduction is good by making close contact with the sample container Therefore, the temperature of the sample container is kept almost the same as that of the thermostatic block. A temperature control unit incorporating a heating / cooling element such as a Peltier element is in close contact with the constant temperature block, and the temperature of the constant temperature block is controlled by controlling the voltage applied to the element (see, for example, Patent Document 1). ).

図３、図４に従来技術の一例を斜視的に示す。なお、図４は図３の中央縦断面を示している。これらの図において、２２は測定する試料であり、３０は試料２２を充填する試料容器、２５は、銅や真鍮などの熱伝導の良い材料で構成されている恒温ブロックである。２８は、試料容器３０を恒温ブロック２５に装填するための凹部であり、２７は発泡スチロール等の断熱材である。断熱材２７は、恒温ブロック２５の温調部が密着している部分を除く表面部分に接して配置されている。２９は、断熱材２７に開いた穴であり、試料容器３０の装填ができるように恒温ブロック２５の凹部２８に対応する部分に空けられている。２３は試料容器３０の蓋であり、２４は、蓋２３に開けられた試料２２の採取のための開口部に詰められた中央付近に切り込みがあるゴム製の栓である。２６は恒温ブロック２５の温度を制御する温調部で、外部からの電気エネルギーにより温度を制御する。なお、図３では電源からの配線等は省略している。   An example of the prior art is shown in perspective in FIGS. FIG. 4 shows a central longitudinal section of FIG. In these figures, 22 is a sample to be measured, 30 is a sample container filled with the sample 22, and 25 is a thermostatic block made of a material having good heat conductivity such as copper or brass. 28 is a recess for loading the sample container 30 into the constant temperature block 25, and 27 is a heat insulating material such as polystyrene foam. The heat insulating material 27 is disposed in contact with the surface portion excluding the portion where the temperature control portion of the constant temperature block 25 is in close contact. Reference numeral 29 denotes a hole opened in the heat insulating material 27, which is formed in a portion corresponding to the concave portion 28 of the thermostatic block 25 so that the sample container 30 can be loaded. Reference numeral 23 denotes a lid of the sample container 30, and reference numeral 24 denotes a rubber stopper having a notch in the vicinity of the center packed in an opening for collecting the sample 22 opened in the lid 23. A temperature control unit 26 controls the temperature of the constant temperature block 25, and controls the temperature by external electric energy. In FIG. 3, wiring from the power source is omitted.

特開平１０−１９２７１９号公報JP-A-10-192719

試料温度を均一且つ一定の温度に保つことが測定精度や再現性に必要であるが、従来技術では、試料容器の蓋の部分が外気に触れていたため、試料容器の蓋に近い部分の試料の温度は外気温に近くなっていた。また一方、従来技術では、試料容器と恒温ブロックは密に接触していたため恒温ブロックに距離的に近い部分の試料の温度は恒温ブロックの温度に近く、前述の蓋に近い部分の試料の温度との間に温度差があるため強い温度勾配が生じ、試料内部でのその温度差に由来する試料の濃度ムラなどが原因となる再現性の無さや測定誤差が生じていた。本発明はこのような問題を解決する試料恒温装置を提供するものである。   Maintaining the sample temperature at a uniform and constant temperature is necessary for measurement accuracy and reproducibility, but in the conventional technology, the lid portion of the sample container is in contact with the outside air. The temperature was close to the outside temperature. On the other hand, in the conventional technique, the sample container and the thermostatic block are in close contact with each other, so the temperature of the sample near the thermostatic block is close to the temperature of the thermostatic block, and the temperature of the sample near the lid described above Due to the temperature difference between them, a strong temperature gradient was generated, and there was a lack of reproducibility and measurement errors caused by the density unevenness of the sample resulting from the temperature difference inside the sample. The present invention provides a sample thermostat that solves such problems.

本発明に係る試料恒温装置は、良熱伝導材にて構成され、試料容器を保持する凹部を有し且つ一定の温度に保持する加熱冷却機構を有する恒温ブロックを内部に備える筐体と、前記恒温ブロックの凹部に保持された試料容器を上部から覆い、試料容器の蓋部分が貫通するように前記凹部に対応する孔が穿設された断熱材からなるカバーと、前記カバーを収容し前記筐体に対して支持部を介して片開きで開閉可能なカバー枠と、を備えたことを特徴とする。従って、試料容器の蓋部分が外気と遮断される。
さらに、試料容器と恒温ブロックの凹部の内側面との間に空気層を設けたものである。従って、試料容器の側面からの熱の出入りを妨げる。
さらに、恒温ブロックの凹部の底部が樹脂で構成されている。従って、試料容器の底面からの熱の出入りを妨げる。
さらに、樹脂からなる恒温ブロックの凹部の底部と温調部との間に空気層を設けたものである。従って、試料容器の底面からの熱の出入りを妨げる。 A sample constant temperature apparatus according to the present invention is composed of a good heat conductive material, has a concave portion for holding a sample container and has a constant temperature block having a heating / cooling mechanism for holding at a constant temperature , A cover made of a heat insulating material that covers the sample container held in the concave part of the thermostatic block from above and has a hole corresponding to the concave part so that the lid part of the sample container penetrates, and a housing that accommodates the cover and contains the cover. And a cover frame that can be opened and closed with a single opening through a support portion . Accordingly, the lid portion of the sample container is blocked from the outside air.
Furthermore, an air layer is provided between the sample container and the inner surface of the recess of the thermostatic block. Accordingly, heat entry and exit from the side surface of the sample container is hindered.
Furthermore, the bottom part of the recessed part of a constant temperature block is comprised with resin. Therefore, heat entry and exit from the bottom surface of the sample container is hindered.
Furthermore, an air layer is provided between the bottom of the concave portion of the constant temperature block made of resin and the temperature control portion. Therefore, heat entry and exit from the bottom surface of the sample container is hindered.

本発明の試料恒温装置は、液体クロマトグラフや生化学分析装置などの分析の分野において、測定結果に対して大きな影響力を持つ試料の温度を均一且つ一定に保つことができる。試料内の温度勾配は濃度ムラを引き起こし測定結果の精度や再現性などの正確な定量の妨げとなる。本発明のカバーを設けることによって、試料温度は外気からの影響を受け難くなる。また同時に、試料容器の側面及び底面を、空気層及び樹脂で断熱しているため、試料の温度勾配を少なくできる。貫通孔があるため従来の分析動作を妨げることなく外気温の影響を防ぎ、試料の温度を均一且つ一定にして、測定精度の向上に寄与する。   The sample thermostat of the present invention can keep the temperature of a sample having a large influence on the measurement result uniform and constant in the field of analysis such as a liquid chromatograph and a biochemical analyzer. The temperature gradient in the sample causes density unevenness and hinders accurate quantification such as accuracy and reproducibility of measurement results. By providing the cover of the present invention, the sample temperature is hardly affected by the outside air. At the same time, the temperature gradient of the sample can be reduced because the side surface and the bottom surface of the sample container are insulated by the air layer and the resin. Since there is a through hole, the influence of the outside air temperature is prevented without interfering with the conventional analysis operation, the temperature of the sample is made uniform and constant, and the measurement accuracy is improved.

本発明は、試料容器の蓋部分が挿入可能な孔が穿設されたカバーを設けた点を特徴とするが、このカバーの設置の仕方としては、試料恒温装置の筐体に対して、係合され、且つ、開閉可能とするのが操作性もよく、最良の形態である。   The present invention is characterized in that a cover having a hole into which the lid portion of the sample container can be inserted is provided. The cover is installed with respect to the housing of the sample thermostat. It is the best mode to be able to be opened and closed with good operability.

図１は本発明の一実施例を斜視的に示す図で、４が本発明のカバーであり、１３は、このカバー４を収納したカバー枠である。１４は、本発明の主要部をなす恒温ブロックや温調部を収容する筐体であり、１５は、カバー枠１３を筐体１４に開閉可能に係合させる支持部である。１６はカバー枠１３に設けられた連結具、１７は筐体１４に設けられた連結用孔であり、筐体１４にカバー枠１３を覆い被せたときに、連結用孔１７に連結具１６が導かれ、結果的に、挿入されてカバー枠１３と筐体１４が完全に係合する。   FIG. 1 is a perspective view showing an embodiment of the present invention. 4 is a cover according to the present invention, and 13 is a cover frame in which the cover 4 is accommodated. Reference numeral 14 denotes a housing that houses a constant temperature block and a temperature control portion that constitute the main part of the present invention. Reference numeral 15 denotes a support portion that engages the cover frame 13 with the housing 14 so as to be opened and closed. Reference numeral 16 denotes a connection tool provided in the cover frame 13, and 17 denotes a connection hole provided in the housing 14. When the cover frame 13 is covered with the housing 14, the connection tool 16 is inserted into the connection hole 17. As a result, the cover frame 13 and the housing 14 are completely engaged with each other.

１９はカバー枠１３の側面に設けられたバックル、２０は筐体１４の側面に設けられたバックル用孔であり、筐体１４にカバー枠１３を覆い被せ完全に閉じたときに、バックル１９をバックル用孔２０に引掛けて止めることによりカバー枠１３と筐体１４は開くことがない。１８は把手であり、容易に全体を持ち運びできるよう設けられている。
２は試料を入れる試料容器であり、頭部の蓋の部分だけが見えている。 19 is a buckle provided on the side surface of the cover frame 13, and 20 is a hole for buckle provided on the side surface of the housing 14. When the cover frame 13 is covered with the housing 14 and completely closed, the buckle 19 is The cover frame 13 and the housing 14 do not open by being hooked and stopped on the buckle hole 20. A handle 18 is provided so that the whole can be easily carried.
Reference numeral 2 denotes a sample container in which a sample is placed, and only the lid portion of the head is visible.

図２は、図１において、筐体１４にカバー枠１３を完全に覆い閉じ、試料容器２を完全に差込んだ時のＸ−Ｘ´線での試料容器２近傍の断面を示す。Ａは外気を示している。
３は試料容器２を下部から保持し且つ温度を一定にするための恒温ブロックであり、筐体１４に収納されている。恒温ブロック３は例えば銅・アルミニウム・真鍮などの熱伝導率の良い材料から形成される。５は温調部である。８は、試料容器２が挿入できる大きさの凹部であり、１２は樹脂ブロックであり、凹部８の底部分を構成し、試料容器２を保持する。Ｂは、試料容器２と恒温ブロック３との間の空気層であり、Ｃは、樹脂ブロック１２と温調部５との間の空気層であり、それぞれ、試料容器２への熱の流入・流出を妨げる。凹部８や樹脂ブロック１２は、複数個の試料容器２を保持するために恒温ブロック３に複数個設けられている。 FIG. 2 shows a cross section in the vicinity of the sample container 2 along the line XX ′ when the cover frame 13 is completely covered and closed in the casing 14 in FIG. 1 and the sample container 2 is completely inserted. A indicates outside air.
Reference numeral 3 denotes a thermostatic block for holding the sample container 2 from below and keeping the temperature constant, and is housed in the housing 14. The thermostatic block 3 is made of a material having good thermal conductivity such as copper, aluminum, and brass. 5 is a temperature control part. Reference numeral 8 denotes a recess having a size into which the sample container 2 can be inserted. Reference numeral 12 denotes a resin block, which constitutes a bottom portion of the recess 8 and holds the sample container 2. B is an air layer between the sample container 2 and the constant temperature block 3, and C is an air layer between the resin block 12 and the temperature control unit 5. Prevent spillage. A plurality of recesses 8 and resin blocks 12 are provided in the thermostatic block 3 in order to hold a plurality of sample containers 2.

１１は、断熱材の板であり、恒温ブロック３の温調部が密着している部分を除く表面部分に接して配置され、恒温ブロック３への熱の出入りを防いでいる。断熱材の板１１は、恒温ブロック３の凹部８と同じ位置に試料容器２の外径と同等径の穴が開いており、試料容器２を恒温ブロック３の凹部８に挿入することができる。
４は、試料容器２を上部から覆い外気からの熱の出入りを防ぐ本発明のカバーである。９は孔であり、カバー４に、複数個設けられている。孔９は、凹部８に保持された試料容器２と対応する位置に設けられ、また、試料容器２の蓋部分の外形に対応して切り欠かれており、試料容器２の蓋部側面を断熱すると同時に、試料容器２の中の試料１を採取できるようになっている。また、カバー枠１３にも、カバー４の孔９に対応する位置に同等の孔を設け、試料容器２の中の試料１を採取できるようになっている。 Reference numeral 11 denotes a heat insulating plate, which is disposed in contact with the surface portion excluding the portion where the temperature control portion of the constant temperature block 3 is in close contact, and prevents heat from entering and exiting the constant temperature block 3. The heat insulating plate 11 has a hole having the same diameter as the outer diameter of the sample container 2 at the same position as the recess 8 of the thermostatic block 3, and the sample container 2 can be inserted into the recess 8 of the thermostatic block 3.
4 is a cover of the present invention that covers the sample container 2 from above and prevents heat from entering and exiting from the outside air. Reference numeral 9 denotes a hole, and a plurality of holes are provided on the cover 4. The hole 9 is provided at a position corresponding to the sample container 2 held in the recess 8, and is cut out corresponding to the outer shape of the lid portion of the sample container 2 to insulate the side surface of the lid portion of the sample container 2. At the same time, the sample 1 in the sample container 2 can be collected. The cover frame 13 is also provided with an equivalent hole at a position corresponding to the hole 9 of the cover 4 so that the sample 1 in the sample container 2 can be collected.

カバー枠１３と筐体１４は、図１のＹ−Ｙ´を軸として片開きに開閉可能に構成され、試料容器２の出し入れを容易にしている。
１は測定する試料。温調部５は、恒温ブロック３の底面に密着して設けられ、内部にはペルチェ素子等の加熱冷却素子が組み込まれている。温調部５は、外部からの電源にて駆動しているが、図１、図２では電源からの配線等の図示は省略している。 The cover frame 13 and the housing 14 are configured to be openable and closable with the YY ′ in FIG. 1 as an axis, so that the sample container 2 can be easily inserted and removed.
1 is a sample to be measured. The temperature control unit 5 is provided in close contact with the bottom surface of the constant temperature block 3, and a heating / cooling element such as a Peltier element is incorporated therein. The temperature control unit 5 is driven by a power source from the outside, but illustration of wiring and the like from the power source is omitted in FIGS. 1 and 2.

６は断熱材であり発泡スチロールや発泡ポリプロピレンや独立発泡断熱材などを用いる。断熱材６には孔９が開いているため試料１の採取を妨げることはない。
また、１０は、支持部材の板であり、断熱材６を接着により固定しており、カバー４を構成している。支持部材の板１０をカバー枠１３に固定することにより、カバー４はカバー枠１３に収納されている。
支持部材の板１０には、断熱材６と同様に試料採取のための孔９が開けられている。７は、試料容器２の蓋であり試料採取のための開口部を有している。２１は、中央に切り込みのあるゴム製の栓で上記開口部に詰められているが、切り込みから吸込用針を挿入できる。
図２は、試料容器２を恒温ブロック３の凹部８に挿入させ、カバー４を恒温ブロック３に完全に覆い被せた状態を示しているが、この状態においては、温調部５からの加熱冷却が恒温ブロック３に熱伝導されそれが試料容器２を介して試料１に熱伝導される。一方、外気からの熱の出入りは断熱材６により妨げられ、尚且つ孔９により試料１の採取を可能にしている。
実施例の支持部材の板１０は、金属の板や樹脂の板を用いる。断熱材の板１１は、発泡スチロールや発泡ポリプロピレンを用いる。
さらに、実施例ではカバー枠１３は筐体１４に対し片開きに開閉できる構造であるが、カバー枠１３を筐体１４から分離させ、筐体１４に対して単に脱着させる構造でもよい。 Reference numeral 6 denotes a heat insulating material, which uses foamed polystyrene, foamed polypropylene, independent foamed heat insulating material, or the like. Since the hole 9 is opened in the heat insulating material 6, the collection of the sample 1 is not hindered.
Reference numeral 10 denotes a plate of a support member, which fixes the heat insulating material 6 by adhesion, and constitutes the cover 4. The cover 4 is accommodated in the cover frame 13 by fixing the support member plate 10 to the cover frame 13.
Similar to the heat insulating material 6, a hole 9 for collecting a sample is formed in the plate 10 of the support member. Reference numeral 7 denotes a lid of the sample container 2, which has an opening for collecting a sample. 21 is a rubber stopper with a notch in the center and is packed in the opening, but a suction needle can be inserted through the notch.
FIG. 2 shows a state in which the sample container 2 is inserted into the recess 8 of the constant temperature block 3 and the cover 4 is completely covered with the constant temperature block 3. In this state, the heating and cooling from the temperature adjustment unit 5 is performed. Is conducted to the constant temperature block 3 and is conducted to the sample 1 through the sample container 2. On the other hand, heat entry / exit from the outside air is hindered by the heat insulating material 6 and the sample 1 can be collected by the hole 9.
As the support member plate 10 of the embodiment, a metal plate or a resin plate is used. The heat insulating plate 11 is made of foamed polystyrene or foamed polypropylene.
Further, in the embodiment, the cover frame 13 can be opened and closed with respect to the housing 14 in a single-opening manner, but the cover frame 13 may be separated from the housing 14 and simply detached from the housing 14.

本発明は液体クロマトグラフや生化学自動分析装置などに利用可能である。   The present invention can be used for liquid chromatographs, biochemical automatic analyzers, and the like.

本発明の一実施例を斜視的に示す図である。It is a figure which shows one Example of this invention perspectively. 図1におけるＸ−Ｘ´線での断面であり、カバー枠１３を閉じた場合の試料容器２の近傍を示している。1. It is a cross section in the XX 'line | wire in FIG. 1, The vicinity of the sample container 2 at the time of closing the cover frame 13 is shown. 従来における試料恒温装置の外観を示す図である。It is a figure which shows the external appearance of the conventional sample thermostat. 従来における試料恒温装置の縦断面を示す図である。It is a figure which shows the longitudinal cross-section of the conventional sample thermostat.

符号の説明Explanation of symbols

１ 試料
２ 試料容器
３ 恒温ブロック
４ カバー
５ 温調部
６ 断熱材
７ 蓋
８ 凹部
９ 孔
１０ 支持部材の板
１１ 断熱材の板
１２ 樹脂ブロック
１３ カバー枠
１４ 筐体
１５ 支持部
１６ 連結具
１７ 連結用孔
１８ 把手
１９ バックル
２０ バックル用孔
２１ 栓
２２ 試料
２３ 蓋
２４ 栓
２５ 恒温ブロック
２６ 温調部
２７ 断熱材
２８ 凹部
２９ 穴
３０ 試料容器
Ａ 外気
Ｂ 空気層
Ｃ 空気層 DESCRIPTION OF SYMBOLS 1 Sample 2 Sample container 3 Constant temperature block 4 Cover 5 Temperature control part 6 Heat insulating material 7 Cover 8 Recessed part 9 Hole 10 Supporting member board 11 Heating material board 12 Resin block 13 Cover frame 14 Housing 15 Supporting part 16 Connecting tool 17 Connection Hole 18 Handle 19 Buckle 20 Buckle hole 21 Plug 22 Sample 23 Lid 24 Plug 25 Constant temperature block 26 Temperature control unit 27 Heat insulating material 28 Recess 29 Hole 30 Sample container A Outside air B Air layer C Air layer

Claims (7)

良熱伝導材にて構成され、試料容器を保持する凹部を有し且つ一定の温度に保持する加熱冷却機構を有する恒温ブロックを内部に備える筐体と、
前記恒温ブロックの凹部に保持された試料容器を上部から覆い、試料容器の蓋部分が貫通するように前記凹部に対応する孔が穿設された断熱材からなるカバーと、
前記カバーを収容し前記筐体に対して支持部を介して片開きで開閉可能なカバー枠と、
を備えたことを特徴とする試料恒温装置。 A housing that is made of a good heat conductive material, has a recess that holds the sample container, and has a thermostatic block inside that has a heating and cooling mechanism that holds the sample container at a constant temperature ;
A cover made of a heat insulating material that covers the sample container held in the recess of the thermostatic block from above, and has a hole corresponding to the recess so that the lid portion of the sample container penetrates;
A cover frame that accommodates the cover and can be opened and closed with a single opening via a support portion with respect to the housing;
A sample thermostatic device comprising: 前記試料容器と前記恒温ブロックの凹部の内側面との間に空気層を設けたことを特徴とする請求項１に記載の試料恒温装置。 Samples thermostatic device according to claim 1, characterized in that a layer of air between the inner surface of the concave portion of the sample container and the isothermal block. 前記恒温ブロックの凹部の底部は樹脂にて構成されていることを特徴とする請求項１に記載の試料恒温装置。 The sample thermostat according to claim 1, wherein the bottom of the recess of the thermostatic block is made of resin. 樹脂からなる恒温ブロックの凹部の底部と温調部との間に空気層を設けたことを特徴とする請求項３に記載の試料恒温装置。   The sample thermostat according to claim 3, wherein an air layer is provided between the bottom of the recess of the thermostatic block made of resin and the temperature control section. 前記カバーは、前記カバーを支持する前記カバー枠に固定されていることを特徴とする請求項１記載の試料恒温装置。 The cover, sample thermostat according to claim 1, characterized in that it is fixed to the cover frame for supporting the cover. 前記支持部とは別に前記筐体と前記カバー枠とを係合する連結部材を備えることを特徴とする請求項１に記載の試料恒温装置。The sample thermostat according to claim 1, further comprising a connecting member that engages the casing and the cover frame separately from the support portion. 前記筐体または前記カバー枠のいずれかに把手を設けたことを特徴とする請求項１に記載の試料恒温装置。The sample thermostat according to claim 1, wherein a handle is provided on either the casing or the cover frame.
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CN108688948A (en) * 2018-05-15 2018-10-23 合肥安为康医学检验有限公司 A kind of portable high-efficiency detection kit

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CN106133499B (en) * 2014-04-22 2019-03-15 株式会社岛津制作所 Heat temperature adjustment specimen holder and the specimen temperature regulating device using it
JPWO2023105627A1 (en) * 2021-12-07 2023-06-15
WO2023195522A1 (en) * 2022-04-07 2023-10-12 株式会社日立ハイテク Automatic analysis device

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