JP2002263402A - Extraction method and extraction device - Google Patents

Extraction method and extraction device

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Publication number
JP2002263402A
JP2002263402A JP2001068053A JP2001068053A JP2002263402A JP 2002263402 A JP2002263402 A JP 2002263402A JP 2001068053 A JP2001068053 A JP 2001068053A JP 2001068053 A JP2001068053 A JP 2001068053A JP 2002263402 A JP2002263402 A JP 2002263402A
Authority
JP
Japan
Prior art keywords
extraction
extraction solvent
container
solid sample
temperature
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
JP2001068053A
Other languages
Japanese (ja)
Inventor
Kohei Urano
紘平 浦野
Original Assignee
Dia Instr:Kk
Terumu:Kk
株式会社ダイアインスツルメンツ
株式会社テルム
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 Dia Instr:Kk, Terumu:Kk, 株式会社ダイアインスツルメンツ, 株式会社テルム filed Critical Dia Instr:Kk
Priority to JP2001068053A priority Critical patent/JP2002263402A/en
Publication of JP2002263402A publication Critical patent/JP2002263402A/en
Pending legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To provide a simple extraction method suitable as the concentrating and recovering means of a slight amount of target components in a solid sample and improved so as to obtain a high extraction rate. SOLUTION: In this extraction method, the solid sample is filled in a container, an extraction solvent is continuously passed from either upper part or lower part of the container and brought into contact with the solid sample, the target components in the solid sample are extracted and the extraction solvent flowing out from the other part of the container is recovered without circulating it. A solvent whose boiling point is in the range of 50 to 20 deg.C is used as the extraction solvent, the temperature of the extraction solvent immediately before being brought into contact with the solid sample is adjusted to a fixed temperature in the range being lower than the boiling point by 10 deg.C or more and the temperature of the solid sample is controlled so as to make the temperature of the extraction solvent present at the upper part of the container higher than the temperature of the extraction solvent present at the lower part by 10 deg.C or less. The passing speed of the extraction solvent is controlled to a fixed superficial linear velocity in the range of 0.5 to 5 cm/minute.

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、抽出方法および抽
出装置に関し、詳しくは、固体試料中に微量存在する目
的成分の濃縮回収手段として好適に使用される、簡易な
抽出方法および抽出装置に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an extraction method and an extraction apparatus, and more particularly, to a simple extraction method and an extraction apparatus suitably used as a means for concentrating and recovering a small amount of a target component present in a solid sample.

【0002】[0002]

【従来の技術】微量成分の分析分野においては、固体試
料中の微量目的成分の濃縮回収手段として、ソックスレ
ー抽出器やそれを改良した各種の抽出器が使用されてい
る。これらの抽出器は、それぞれに特徴を有するもの
の、抽出溶剤のリフラックスによる循環使用を基本的な
構成としている。しかしながら、この様な従来の抽出器
は抽出速度が遅く抽出操作に長時間を要するという問題
がある。
2. Description of the Related Art In the field of analysis of trace components, a Soxhlet extractor and various types of improved Soxhlet extractors have been used as means for concentrating and recovering trace target components in solid samples. Although each of these extractors has its own characteristics, the extractor has a basic configuration that is circulated and used by the reflux of the extraction solvent. However, such a conventional extractor has a problem that the extraction speed is slow and the extraction operation takes a long time.

【0003】[0003]

【発明が解決しようとする課題】本発明は、上記実情に
鑑みなされたものであり、その目的は、固体試料中の微
量目的成分の濃縮回収手段として好適であって、高い抽
出速度が得られる様に改良された簡易な抽出方法および
抽出装置を提供することにある。
SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned circumstances, and has as its object the purpose of being suitable as a means for concentrating and recovering a trace amount of a target component in a solid sample, whereby a high extraction rate can be obtained. It is an object of the present invention to provide a simple extraction method and an extraction device improved as described above.

【0004】[0004]

【課題を解決するための手段】すなわち、本発明の第1
の要旨は、容器に固体試料を充填し、当該容器の上部ま
たは下部の一方から抽出溶剤を連続的に通液させて固体
試料と接触させ、固体試料中の目的成分を抽出して当該
容器の他方から流出する抽出溶剤を循環せずに回収する
抽出方法であって、抽出溶剤として沸点が50〜200
℃範囲の抽出溶剤を使用し、固体試料に接触する直前の
抽出溶剤の温度をその沸点より10℃以上低い範囲の一
定の温度とし、当該容器の上部に存在する抽出溶剤の温
度が下部に存在する抽出溶剤の温度より10℃以内の範
囲で高くなる様に固体試料の温度を制御し、抽出溶剤の
通液速度を0.5〜5cm/分の範囲の一定の空筒線流
速に制御することを特徴とする抽出方法に存する。
That is, the first aspect of the present invention is as follows.
The point is that a container is filled with a solid sample, an extraction solvent is continuously passed from one of the upper and lower portions of the container to make contact with the solid sample, the target component in the solid sample is extracted, and the An extraction method for recovering an extraction solvent flowing out of the other without circulation, wherein the extraction solvent has a boiling point of 50 to 200.
Using an extraction solvent in the range of ° C, the temperature of the extraction solvent immediately before coming into contact with the solid sample is set to a certain temperature in the range of at least 10 ° C lower than its boiling point, and the temperature of the extraction solvent at the top of the container is at the bottom. The temperature of the solid sample is controlled so as to be higher than the temperature of the extraction solvent within 10 ° C., and the flow rate of the extraction solvent is controlled to a constant cylinder linear flow rate in the range of 0.5 to 5 cm / min. The extraction method is characterized in that:

【0005】そして、本発明の第2の要旨は、固体試料
充填用容器(1)、当該容器の周囲に配置された容器加
熱機構(2)、抽出溶剤リザーバーに連結され且つ容器
(1)の上部または下部の一方に接続された抽出溶剤供
給配管(3)、当該抽出溶剤供給配管の少なくとも容器
側先端の周囲に配置された配管加熱機構(5)、容器
(1)の他方に接続された抽出液導出配管(6)、固体
試料充填用容器(1)に抽出溶剤リザーバー中の抽出溶
剤を供給する定流量送液機構から主として構成されて成
ることを特徴とする抽出装置に存する。
[0005] A second aspect of the present invention is to provide a container (1) for filling a solid sample, a container heating mechanism (2) disposed around the container, and an extraction solvent reservoir connected to the container (1). An extraction solvent supply pipe (3) connected to one of the upper or lower part, a pipe heating mechanism (5) arranged at least around the tip of the extraction solvent supply pipe on the container side, and connected to the other of the container (1). An extractor is characterized by being mainly constituted by an extraction liquid outlet pipe (6) and a constant flow rate liquid feeding mechanism for supplying an extraction solvent in an extraction solvent reservoir to a solid sample filling container (1).

【0006】[0006]

【発明の実施の形態】先ず、説明の便宜上、本発明の抽
出装置について説明する。図1は、本発明の好ましい態
様の抽出装置の一例の説明図である。図1に示す抽出装
置は、抽出溶剤の通液方式がダウンフロー方式になさ
れ、固体試料充填用容器(1)、容器加熱機構(2)、
抽出溶剤供給配管(3)、固体試料充填用容器(1)に
抽出溶剤リザーバー中の抽出溶剤を供給する定流量送液
機構としての定流量ポンプ(4)、配管加熱機構
(5)、抽出液導出配管(6)から主として構成され
る。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS First, for convenience of explanation, an extraction apparatus of the present invention will be described. FIG. 1 is a diagram illustrating an example of an extraction device according to a preferred embodiment of the present invention. The extraction apparatus shown in FIG. 1 employs a down-flow method in which an extraction solvent flows, and includes a solid sample filling container (1), a container heating mechanism (2),
Extraction solvent supply pipe (3), constant flow pump (4) as a constant flow rate liquid supply mechanism for supplying extraction solvent in extraction solvent reservoir to solid sample filling container (1), pipe heating mechanism (5), extract It is mainly composed of the outlet pipe (6).

【0007】固体試料充填用容器(1)は、ガラス、プ
ラスチックス、金属などの適宜の材質から成る円筒体で
構成されている。そして、容器(1)の底部は、固液分
離可能とするためにフィルター構造(図示せず)となさ
れている。斯かるフィルター構造は、後述する抽出液導
出配管(5)の内部に備えることも出来る。なお、符号
(11)は固体試料を表す。
The solid sample filling container (1) is formed of a cylindrical body made of a suitable material such as glass, plastics, and metal. The bottom of the container (1) has a filter structure (not shown) to enable solid-liquid separation. Such a filter structure can also be provided inside the extraction liquid outlet pipe (5) described later. The symbol (11) indicates a solid sample.

【0008】容器加熱機構(2)は、容器の周囲に配置
され、ブロックヒーターで構成されている。二重構造の
容器を使用し、熱媒体を循環するジャケット方式の加熱
機構も採用することが出来る。そして、容器加熱機構
(2)は、図示を省略した温度制御機構によって制御さ
れ、容器を一定温度に保持する。
[0008] The container heating mechanism (2) is arranged around the container and is constituted by a block heater. A jacket-type heating mechanism that uses a double-structured container and circulates a heat medium can also be employed. The container heating mechanism (2) is controlled by a temperature control mechanism (not shown) to maintain the container at a constant temperature.

【0009】抽出溶剤供給配管(3)は、抽出溶剤リザ
ーバーに連結され且つ容器(1)の上部に接続されてい
る。図1に例示した抽出装置の場合、2種類の抽出溶剤
の切り替え使用を可能にするため、使用抽出溶剤リザー
バーは、符号(6a)及び(6b)で表記されて2個設
けられている。各抽出溶剤リザーバー(6a)及び(6
b)には、例えば、非親水性抽出溶剤と親水性溶剤とを
それぞれ収容させ、親水性溶剤を通液させて固体試料の
脱水を行なった後に非親水性抽出溶剤を通液させて抽出
を行うことが出来る。なお、抽出溶剤供給配管(3)
は、容器(1)と同様の材質で構成される。
The extraction solvent supply pipe (3) is connected to the extraction solvent reservoir and connected to the upper part of the container (1). In the case of the extraction device illustrated in FIG. 1, two extraction solvent reservoirs are provided, denoted by reference numerals (6a) and (6b), in order to enable switching use of two types of extraction solvents. Each extraction solvent reservoir (6a) and (6
In b), for example, a non-hydrophilic extraction solvent and a hydrophilic solvent are respectively accommodated, the hydrophilic solvent is passed through, and the solid sample is dehydrated. You can do it. In addition, extraction solvent supply piping (3)
Is made of the same material as the container (1).

【0010】定流量ポンプ(4)は、抽出溶剤供給配管
(3)の途中に配置され、ゼニスポンプ等で構成され
る。図1に例示した抽出装置の場合、抽出溶剤リザーバ
ー(6a)及び(6b)に対して共通する一基の定流量
ポンプ(4)が設けられているが、各抽出溶剤リザーバ
ー毎に定流量ポンプを設けてもよい。
The constant flow pump (4) is arranged in the middle of the extraction solvent supply pipe (3) and is composed of a Zenith pump or the like. In the case of the extraction device illustrated in FIG. 1, a single constant flow pump (4) is provided in common for the extraction solvent reservoirs (6a) and (6b), but a constant flow pump is provided for each extraction solvent reservoir. May be provided.

【0011】配管加熱機構(5)は、抽出溶剤供給配管
(3)の少なくとも容器(1)側先端の周囲に配置さ
れ、リボンヒーターで構成されている。配管加熱機構と
しては、前述のジャケット方式の加熱機構も採用するこ
とが出来る。配管加熱機構(4)は、図示を省略した温
度制御機構によって制御され、容器(1)に充填される
固体試料と接触する直前の抽出溶剤の温度を一定温度に
保持する。
The pipe heating mechanism (5) is arranged at least around the tip of the extraction solvent supply pipe (3) on the container (1) side, and is constituted by a ribbon heater. As the pipe heating mechanism, the above-described jacket-type heating mechanism can also be employed. The piping heating mechanism (4) is controlled by a temperature control mechanism (not shown) to maintain the temperature of the extraction solvent immediately before coming into contact with the solid sample filled in the container (1) at a constant temperature.

【0012】抽出液導出配管(6)は、容器(1)の底
部に接続され、目的成分を抽出した抽出液を受器(7)
に導く。なお、抽出溶剤供給配管(3)は、容器(1)
と同様の材質で構成される。また、抽出液が貯留された
受器(7)は、抽出液導出配管(6)から取り外され、
必要に応じて次の濃縮工程に移送される。
The extraction liquid outlet pipe (6) is connected to the bottom of the vessel (1), and receives the extraction liquid from which the target component has been extracted (7).
Lead to. The extraction solvent supply pipe (3) is connected to the container (1)
It is made of the same material as. Further, the receiver (7) in which the extract is stored is detached from the extract lead-out pipe (6),
It is transferred to the next concentration step as needed.

【0013】本発明においては、固体試料充填用容器
(1)に抽出溶剤リザーバー中の抽出溶剤を供給する定
流量送液機構として、抽出溶剤供給配管(3)の途中に
配置された定流量ポンプ(4)に代えて、抽出溶剤リザ
ーバーの内部にガス圧力を作用させる加圧手段を採用す
ることも出来る。斯かる加圧手段は、例えば圧力調節弁
を備えた加圧ガス供給配管という簡単な設備によって達
成され、圧力調節弁の調節により定流量送液が可能とな
る。しかも、抽出溶剤リザーバーに収容された所定量の
抽出溶剤の送液が終了後に引き続き加圧ガスを供給する
ならば、固体試料充填用容器(1)中の固体試料(1
1)に残存する抽出溶剤をブローイングにより回収する
ことが出来る。
In the present invention, as a constant flow rate liquid supply mechanism for supplying the extraction solvent in the extraction solvent reservoir to the solid sample filling container (1), a constant flow rate pump disposed in the middle of the extraction solvent supply pipe (3). Instead of (4), a pressurizing means for applying a gas pressure to the inside of the extraction solvent reservoir may be employed. Such a pressurizing means is achieved by a simple equipment such as a pressurized gas supply pipe provided with a pressure control valve, and a constant flow rate can be supplied by adjusting the pressure control valve. In addition, if the pressurized gas is continuously supplied after the completion of the feeding of the predetermined amount of the extraction solvent contained in the extraction solvent reservoir, the solid sample (1) in the solid sample filling container (1) is
The extraction solvent remaining in 1) can be recovered by blowing.

【0014】本発明の抽出装置は、上記の様に構成さ
れ、次の様な特徴を有する。すなわち、本発明の抽出装
置は、抽出溶剤のリフラックスによる循環使用を前提と
したソックスレー抽出器とは基本的に異なり、抽出溶剤
の循環使用を行わない。要するに、本発明の抽出装置の
場合、抽出溶剤は、固体試料と所謂ワンパス接触する。
また、本発明の抽出装置は、容器加熱機構(2)及び配
管加熱機構(5)により、高められた温度での抽出が可
能となる。
The extraction device of the present invention is configured as described above and has the following features. That is, the extraction apparatus of the present invention is basically different from a Soxhlet extractor on the assumption that the extraction solvent is circulated by reflux, and does not use the extraction solvent circulated. In short, in the case of the extraction device of the present invention, the extraction solvent comes into so-called one-pass contact with the solid sample.
Moreover, the extraction apparatus of the present invention enables extraction at an elevated temperature by the container heating mechanism (2) and the pipe heating mechanism (5).

【0015】固体からの抽出は目的成分の拡散速度に依
存する。本発明の抽出装置の場合、固体試料は常にフレ
ッシュな抽出溶剤と接触することになり、拡散速度を高
めるための濃度勾配が常に高く保持される。また、温度
が10℃上がる毎に拡散速度は約1.4倍に高められ
る。従って、仮に抽出温度を20℃から80℃に高めた
場合は7〜8倍拡散速度が高くなる。なお、本発明の抽
出装置の使用方法は後述の本発明の抽出方法で説明す
る。
[0015] Extraction from a solid depends on the diffusion rate of the target component. In the case of the extraction device of the present invention, the solid sample is always in contact with the fresh extraction solvent, and the concentration gradient for increasing the diffusion rate is always kept high. Also, the diffusion rate is increased about 1.4 times every time the temperature rises by 10 ° C. Therefore, if the extraction temperature is increased from 20 ° C. to 80 ° C., the diffusion rate increases 7 to 8 times. The method of using the extraction device of the present invention will be described later in the extraction method of the present invention.

【0016】また、本発明においては、図示していない
が、上記のダウンフロー方式に代え、抽出溶剤の通液方
向が下方から上方のアップフロー方式にすることも出来
る。この場合、抽出溶剤供給配管(3)は容器(1)の
底部に接続され、抽出液導出配管(6)は容器(1)の
上部に接続される。
In the present invention, although not shown, an upflow system in which the direction of flow of the extraction solvent is upward from below may be used instead of the above downflow system. In this case, the extraction solvent supply pipe (3) is connected to the bottom of the vessel (1), and the extraction liquid outlet pipe (6) is connected to the top of the vessel (1).

【0017】次に、本発明の抽出方法について説明す
る。本発明の抽出方法は固体試料に適用される。固体試
料としては、焼却灰、土壌、汚泥、生物試料、食品の
他、排ガスや大気、排水や環境水などから有機物質を捕
集した吸着剤、ろ剤などの固体試料が挙げられる。そし
て、本発明においては、抽出溶剤の通液方式として、ダ
ウンフロー方式またはアップフロー方式の何れであって
もよい。ダウンフロー方式の場合は例えば前記の抽出装
置を使用して次の様に行うことが出来る。
Next, the extraction method of the present invention will be described. The extraction method of the present invention is applied to a solid sample. Examples of the solid sample include solid samples such as incineration ash, soil, sludge, biological samples, and foods, as well as adsorbents and filter media that collect organic substances from exhaust gas, air, wastewater, environmental water, and the like. In the present invention, either a downflow method or an upflow method may be used as a method for passing the extraction solvent. In the case of the downflow method, for example, the above-mentioned extraction device can be used to carry out the following.

【0018】本発明の抽出方法では、容器(1)に固体
試料(11)を充填し、容器(1)の上部から抽出溶剤
を連続的に通液させて固体試料(11)と接触させ、固
体試料(11)中の目的成分を抽出する。そして、容器
(1)の下部から流出する抽出溶剤を循環せずに回収す
る。従って、前述の通り、固体試料(11)は常にフレ
ッシュな抽出溶剤と接触することになり、拡散速度を高
めるための濃度勾配が常に高く保持される。
In the extraction method of the present invention, the container (1) is filled with the solid sample (11), and the extraction solvent is continuously passed through the upper portion of the container (1) to contact the solid sample (11). The target component in the solid sample (11) is extracted. Then, the extraction solvent flowing out from the lower part of the container (1) is recovered without being circulated. Therefore, as described above, the solid sample (11) always comes into contact with the fresh extraction solvent, and the concentration gradient for increasing the diffusion rate is always kept high.

【0019】本発明の抽出方法では、上記の抽出溶剤と
して、沸点が50〜200℃の範囲の抽出溶剤を使用す
る。沸点が50℃未満の抽出溶剤を使用した場合は、後
述する様に抽出温度を高めた際に加圧状態となり易く操
作性に劣り、また、沸点が200℃を超える抽出溶剤を
使用した場合は、抽出後の濃縮操作が困難となる。抽出
溶剤の好ましい沸点は、60〜200℃である。
In the extraction method of the present invention, an extraction solvent having a boiling point in the range of 50 to 200 ° C. is used as the above-mentioned extraction solvent. When an extraction solvent having a boiling point of less than 50 ° C. is used, when the extraction temperature is increased, a pressurized state is likely to occur when the extraction temperature is increased, and the operability is poor, and when an extraction solvent having a boiling point of more than 200 ° C. is used, In addition, the concentration operation after extraction becomes difficult. The preferred boiling point of the extraction solvent is from 60 to 200C.

【0020】抽出溶剤は、非親水性抽出溶剤と親水性抽
出溶剤とに大別される。これらは、抽出の目的成分に応
じて適宜選択される。非親水性抽出溶剤としては、例え
ば、ベンゼン、トルエン、キシレン等の芳香族炭化水
素、クロロホルム、ジクロロエタン等のハロゲン化炭化
水素などが挙げられ、親水性抽出溶剤としては、例え
ば、メタノール、エタノール、プロパノール等の低級ア
ルコール又はアセトン等の低級ケトンが挙げられる。
The extraction solvent is roughly classified into a non-hydrophilic extraction solvent and a hydrophilic extraction solvent. These are appropriately selected according to the target component of the extraction. Examples of the non-hydrophilic extraction solvent include, for example, aromatic hydrocarbons such as benzene, toluene, and xylene, and halogenated hydrocarbons such as chloroform and dichloroethane. Examples of the hydrophilic extraction solvent include methanol, ethanol, and propanol. And lower ketones such as acetone.

【0021】一般に、抽出の目的成分としては非親水性
抽出溶剤で抽出されるものが多く、従って、抽出溶剤と
しては非親水性抽出溶剤が使用される場合が多い。斯か
る場合、本発明の好ましい態様においては、親水性溶剤
を通液させて固体試料の脱水を行なった後に非親水性抽
出溶剤を通液させて目的成分の抽出を行う。これによ
り、固体試料(11)中の水分が脱水されて固体試料と
非親水性抽出溶剤との接触が良好となり、その後の抽出
効率が高められる。
In general, the target component of the extraction is often extracted with a non-hydrophilic extraction solvent, and therefore, a non-hydrophilic extraction solvent is often used as the extraction solvent. In such a case, in a preferred embodiment of the present invention, the solid component is dehydrated by passing a hydrophilic solvent, and then the target component is extracted by passing a non-hydrophilic extraction solvent. As a result, the water in the solid sample (11) is dehydrated, and the contact between the solid sample and the non-hydrophilic extraction solvent is improved, and the subsequent extraction efficiency is increased.

【0022】抽出溶剤リザーバー(6a)及び(6b)
にそれぞれ貯蔵された親水性溶剤および非親水性抽出溶
剤は、順次に切り替えられ、定流量ポンプ(4)によ
り、抽出溶剤供給配管(3)から容器(1)に供給され
る。なお、親水性溶剤による脱水処理は、加熱乾燥では
目的成分が揮発または変質する様な場合に特に有効であ
る。しかも、斯かる問題を考慮して行われる風乾より遥
かに効率的である。
Extraction solvent reservoirs (6a) and (6b)
The hydrophilic solvent and the non-hydrophilic extraction solvent respectively stored in are sequentially switched and supplied to the vessel (1) from the extraction solvent supply pipe (3) by the constant flow pump (4). The dehydration treatment with a hydrophilic solvent is particularly effective when the target component is volatilized or deteriorated by heating and drying. Moreover, it is much more efficient than air drying performed in consideration of such a problem.

【0023】本発明の抽出方法においては、固体試料
(11)に接触する直前の抽出溶剤の温度をその沸点よ
り10℃以上低い範囲の一定の温度とし、容器(1)の
上部に存在する抽出溶剤の温度が下部に存在する抽出溶
剤の温度より10℃以内の範囲で高くなる様に固体試料
(11)の温度を制御する。すなわち、ダウンフロー方
式の場合は、固体試料(11)の温度を上記の抽出溶剤
の温度と同じ又はそれより10℃低い温度範囲の一定の
温度に制御する。これにより、抽出溶剤の温度は初めと
同じか又は冷却されて容器(1)の底部から抜き出され
る。アップフロー方式の場合は、固体試料(11)の温
度を上記の抽出溶剤の温度と同じ又はそれより10℃高
い温度範囲の一定の温度に制御する。これにより、初め
と同じか又は加温されて容器(1)の上部から抜き出さ
れる。これらの温度制御は、容器加熱機構(2)及び配
管加熱機構(5)によって行われる。
In the extraction method of the present invention, the temperature of the extraction solvent immediately before coming into contact with the solid sample (11) is set at a constant temperature lower than its boiling point by 10 ° C. or more, and the extraction solvent existing in the upper part of the container (1) is removed. The temperature of the solid sample (11) is controlled so that the temperature of the solvent becomes higher than the temperature of the extraction solvent present in the lower part within a range of 10 ° C or less. That is, in the case of the downflow method, the temperature of the solid sample (11) is controlled to a constant temperature in the temperature range equal to or lower than the temperature of the above-mentioned extraction solvent by 10 ° C. As a result, the temperature of the extraction solvent is the same as at the beginning or is cooled and the extraction solvent is withdrawn from the bottom of the container (1). In the case of the up-flow method, the temperature of the solid sample (11) is controlled to a constant temperature equal to or higher by 10 ° C. than the temperature of the extraction solvent. Thereby, it is extracted from the upper part of the container (1) with the same temperature as that at the beginning or heated. These temperature controls are performed by the container heating mechanism (2) and the pipe heating mechanism (5).

【0024】抽出溶剤および固体試料の温度を上記の様
な沸点以下の温度に制御することにより、常圧状態での
抽出操作を可能にしつつ可及的に高められた温度での抽
出が可能となり、目的成分の拡散速度が高められる。ま
た、固体試料の温度を上記の様に制御することにより、
固体試料に接触した抽出溶剤の温度変化(密度変化)に
よる対流(すなわち、ダウンフロー方式の場合に問題と
なる部分的なアップフローやアップフロー方式の場合に
問題となる部分的なダウンフロー)が阻止される。換言
すれば、抽出溶剤は、ピストン流の様に流れてバックミ
キシングが防止されるため、固体試料(11)が常にフ
レッシュな抽出溶剤と接触するという条件が極めて高度
に達成される。これらの温度制御は、特に非親水性抽出
溶剤を通液させて固体試料と接触させる際に重要とな
る。
By controlling the temperature of the extraction solvent and the solid sample to a temperature below the boiling point as described above, it is possible to perform extraction at normal pressure and to perform extraction at as high a temperature as possible. The diffusion rate of the target component is increased. Also, by controlling the temperature of the solid sample as described above,
Convection due to temperature change (density change) of the extraction solvent in contact with the solid sample (that is, partial upflow which is a problem in the case of the downflow method or partial downflow which is a problem in the case of the upflow method) Will be blocked. In other words, since the extraction solvent flows like a piston flow and back mixing is prevented, the condition that the solid sample (11) is always in contact with the fresh extraction solvent is achieved at a very high level. These temperature controls are particularly important when a non-hydrophilic extraction solvent is passed through and brought into contact with a solid sample.

【0025】本発明の抽出方法においては、抽出溶剤の
通液速度を0.5〜5cm/分の範囲の一定の空筒線流
速に制御する。斯かる条件により、固体表面に存在する
目的成分が動的に剥離されて抽出速度が高められる。斯
かる観点から、抽出溶剤の通液速度は速いほど好ましい
が、5cm/分を超える通液速度は、使用する抽出溶剤
の量が多くなり過ぎて経済的ではない。抽出溶剤の通液
速度の好ましい範囲は1〜3cm/分である。抽出溶剤
の通液速度の条件は、特に非親水性抽出溶剤と固体試料
と接触させる際に重要となる。
In the extraction method of the present invention, the flow rate of the extraction solvent is controlled to a constant hollow linear velocity in the range of 0.5 to 5 cm / min. Under such conditions, the target component present on the solid surface is dynamically exfoliated and the extraction speed is increased. From this point of view, the higher the flow rate of the extraction solvent, the better, but the flow rate exceeding 5 cm / min is not economical because the amount of the extraction solvent to be used becomes too large. The preferred range of the flow rate of the extraction solvent is 1 to 3 cm / min. The conditions for the flow rate of the extraction solvent are particularly important when the non-hydrophilic extraction solvent is brought into contact with the solid sample.

【0026】因に、親水性溶剤を通液させて固体試料の
脱水を行なった後に非親水性抽出溶剤を通液させて目的
成分の抽出を行う場合の抽出溶剤の一般的な使用量(固
体試料の充填量当たりの量)は、親水性溶剤2〜15
倍、非親水性溶剤5〜40倍である。
The amount of the extraction solvent generally used (solids) when a hydrophilic sample is passed through to dehydrate a solid sample and then a non-hydrophilic extraction solvent is passed to extract the target component The amount per sample filling) is 2 to 15 of the hydrophilic solvent.
Times, 5 to 40 times the non-hydrophilic solvent.

【0027】[0027]

【実施例】以下、本発明を試験例および実施例により更
に詳細に説明するが、本発明は、その要旨を超えない限
り、以下の実施例に限定されるものではない。なお、以
下の実施例においては、図1に示すのと同様の抽出装置
を使用した。
EXAMPLES The present invention will be described in more detail with reference to Test Examples and Examples, which should not be construed as limiting the scope of the present invention. In the following examples, the same extraction device as that shown in FIG. 1 was used.

【0028】試験例1 抽出温度による抽出量の影響を検討するため次の試験を
行った。ごみ焼却施設の集塵機から採取した飛灰A約1
0gを100mlの2M塩酸でカルシウム分などを溶解
処理した後に濾過して固体試料を調製した。容器(1)
に調製した固体試料5mlを充填し、定流量ポンプ
(4)により、抽出溶剤リザーバー(6a)及び(6
b)にそれぞれ貯蔵されたエタノール及びトルエンを順
次に切り替えて抽出溶剤供給配管(3)から容器(1)
に供給しダイオキシン類を抽出した。エタノールの供給
量は30ml、トルエンの供給量は150mlとした。
Test Example 1 The following test was conducted to examine the effect of the extraction temperature on the extraction temperature. Approximately 1 fly ash A collected from a dust collector at a waste incineration facility
0 g was dissolved in 100 ml of 2M hydrochloric acid to dissolve calcium and the like, and then filtered to prepare a solid sample. Container (1)
5 ml of the prepared solid sample, and the extraction solvent reservoirs (6a) and (6)
The ethanol and toluene respectively stored in b) are sequentially switched, and the extraction solvent supply pipe (3) is connected to the container (1).
And dioxins were extracted. The supply amount of ethanol was 30 ml, and the supply amount of toluene was 150 ml.

【0029】そして、トルエン(常圧沸点:110℃)
の供給の際、配管加熱機構(5)により、トルエンの温
度を室温(約20℃)から90℃まで変更した。ただ
し、トルエンの空筒線速度は1cm/分とした。結果を表
1に示す。
Then, toluene (normal pressure boiling point: 110 ° C.)
During the supply, the temperature of toluene was changed from room temperature (about 20 ° C.) to 90 ° C. by the piping heating mechanism (5). However, the linear velocity of the hollow cylinder of toluene was 1 cm / min. Table 1 shows the results.

【0030】[0030]

【表1】 [Table 1]

【0031】表1に示す結果から明らかな様に、トルエ
ンの温度を高くするにつれて抽出量が増え、加熱するこ
とによって効率的にダイオキシン類を抽出できる。ま
た、80℃と90℃とでは差がなく、トルエンの温度を
80℃程度に加熱すればよいことが分かった。
As is clear from the results shown in Table 1, the amount of extraction increases as the temperature of toluene increases, and dioxins can be efficiently extracted by heating. In addition, there was no difference between 80 ° C. and 90 ° C., and it was found that the temperature of toluene should be heated to about 80 ° C.

【0032】試験例2 ダイオキシン類の抽出に必要な抽出溶剤量を検討するた
め次の試験を行った。ごみ焼却施設の集塵機から採取し
た飛灰B約10gを100mlの2M塩酸でカルシウム
分などを溶解処理した後に濾過して固体試料を調製し
た。容器(1)に調製した固体試料5mlを充填し、試
験例1と同様にしてエタノール及びトルエンを容器
(1)に供給しダイオキシン類を抽出した。エタノール
の供給量は30ml、トルエンの供給量は250mlと
した。また、トルエンの温度は80℃、空筒線速度は1
cm/分とした。そして、トルエンの抽出液を50ml毎
に分取した。結果を表2に示す。
Test Example 2 The following test was conducted to examine the amount of extraction solvent required for extracting dioxins. Approximately 10 g of fly ash B collected from a dust collector in a refuse incineration facility was treated with 100 ml of 2M hydrochloric acid to dissolve calcium and the like, followed by filtration to prepare a solid sample. Container (1) was filled with 5 ml of the prepared solid sample, and ethanol and toluene were supplied to container (1) to extract dioxins in the same manner as in Test Example 1. The supply amount of ethanol was 30 ml, and the supply amount of toluene was 250 ml. The temperature of toluene is 80 ° C and the linear velocity of the cylinder is 1
cm / min. Then, the extract of toluene was fractionated every 50 ml. Table 2 shows the results.

【0033】[0033]

【表2】 [Table 2]

【0034】表2に示す結果から明らかな様に、何れの
ダイオキシン類も抽出溶剤量が試料充填体積の約20倍
の100mlで略97%抽出でき、約30倍の150m
lで略100%抽出されることが分かった。
As is clear from the results shown in Table 2, almost all dioxins can be extracted by about 97% with 100 ml of the extraction solvent amount which is about 20 times the sample filling volume, and about 30 times with 150 m.
It was found that about 100% was extracted with l.

【0035】実施例1 ごみ焼却施設の集塵機から採取した飛灰C約10gを1
00mlの2M塩酸でカルシウム分などを溶解処理した
後に濾過して固体試料を調製した。容器(1)に調製し
た固体試料5mlを充填し、試験例1と同様にしてエタ
ノール及びトルエンを容器(1)に供給しダイオキシン
類を抽出した。エタノールの供給量は30ml、トルエ
ンの供給量は150mlとした。また、トルエンの温度
は80℃、空筒線速度は1cm/分とした(通液時間30
分)。結果を表3に示す。
Example 1 About 10 g of fly ash C collected from a dust collector of a refuse incineration facility was
After dissolving calcium and the like with 00 ml of 2M hydrochloric acid, the mixture was filtered to prepare a solid sample. Container (1) was filled with 5 ml of the prepared solid sample, and ethanol and toluene were supplied to container (1) to extract dioxins in the same manner as in Test Example 1. The supply amount of ethanol was 30 ml, and the supply amount of toluene was 150 ml. The temperature of the toluene was 80 ° C., and the linear velocity of the hollow cylinder was 1 cm / min.
Minutes). Table 3 shows the results.

【0036】比較例1 実施例1と同様の固体試料(約10g)を一昼夜風乾
後、ジクロロメタン300mlを使用し、ソックスレー
抽出器により、16時間ダイオキシン類を抽出した。結
果を表3に示す。
Comparative Example 1 The same solid sample (about 10 g) as in Example 1 was air-dried all day and night, and dioxins were extracted with a Soxhlet extractor using 300 ml of dichloromethane for 16 hours. Table 3 shows the results.

【0037】実施例2 固体試料として産業廃棄物焼却施設周辺の汚染された土
壌Aを使用した。容器(1)に15ml(約10g)の
固体試料を充填し、実施例1と同様にしてエタノール及
びトルエンを容器(1)に供給しダイオキシン類を抽出
した。エタノールの供給量は60ml、トルエンの供給
量は150mlとした。また、トルエンの温度は80
℃、空筒線速度は2cm/分とした(通液時間25分)。
結果を表3に示す。
Example 2 Contaminated soil A around an industrial waste incineration facility was used as a solid sample. The container (1) was filled with 15 ml (about 10 g) of a solid sample, and ethanol and toluene were supplied to the container (1) to extract dioxins in the same manner as in Example 1. The supply amount of ethanol was 60 ml, and the supply amount of toluene was 150 ml. The temperature of toluene is 80
° C and the linear velocity of the hollow cylinder were 2 cm / min (liquid passing time: 25 minutes).
Table 3 shows the results.

【0038】比較例2 実施例2と同様の固体試料(約10g)を一昼夜風乾
後、ジクロロメタン300mlを使用し、ソックスレー
抽出器により、16時間ダイオキシン類を抽出した。結
果を表3に示す。
Comparative Example 2 A solid sample (about 10 g) similar to that in Example 2 was air-dried all day and night, and dioxins were extracted with a Soxhlet extractor for 16 hours using 300 ml of dichloromethane. Table 3 shows the results.

【0039】[0039]

【表3】 [Table 3]

【0040】表3に示す結果から明らかな様に、抽出溶
剤の循環使用を行わない本発明の抽出方法は、抽出溶剤
の循環使用を行うソックスレー抽出法(循環方式)に比
し、約10〜20%抽出量が多く、抽出効果が高い。ま
た、本発明の抽出方法では、従来法に比べて、抽出溶剤
量を約1/2、脱水と抽出に要する時間を約1/30以
下にすることが出来る。
As is clear from the results shown in Table 3, the extraction method of the present invention in which the extraction solvent is not recycled is about 10 to 10 times less than the Soxhlet extraction method (circulation method) in which the extraction solvent is recycled. The extraction amount is large by 20%, and the extraction effect is high. Further, in the extraction method of the present invention, the amount of the extraction solvent can be reduced to about 1/2 and the time required for dehydration and extraction can be reduced to about 1/30 or less as compared with the conventional method.

【0041】実施例3 ガラス繊維濾紙を付けたハイボリュームエアサンプラー
で幹線道路近くの大気を採取し、当該濾紙をそれぞれ2
分割し、半分の濾紙を小さく切って固体試料を調製し
た。容器(1)に約30mlの固体試料を充填し、試験
例1と同様にしてエタノール及びトルエンを容器(1)
に供給し多環芳香族炭化水素類を抽出した。エタノール
の供給量は60ml、トルエンの供給量は150mlと
した。また、トルエンの温度は80℃、空筒線速度は1
cm/分とした(通液時間50分)。結果を表4に示す。
Example 3 The air near the main road was sampled with a high-volume air sampler equipped with a glass fiber filter paper, and the filter paper was applied to each of the samples.
A solid sample was prepared by splitting and cutting half of the filter paper into small pieces. A container (1) was filled with about 30 ml of a solid sample, and ethanol and toluene were placed in the container (1) in the same manner as in Test Example 1.
And extracted polycyclic aromatic hydrocarbons. The supply amount of ethanol was 60 ml, and the supply amount of toluene was 150 ml. The temperature of toluene is 80 ° C and the linear velocity of the cylinder is 1
cm / min (flow time: 50 minutes). Table 4 shows the results.

【0042】比較例3 実施例3で得た残りの半分の濾紙を固体試料として使用
した。JIS法に従って脱水せずに使用した。ソックス
レー抽出器により、300mlのトルエンで16時間に
亘り多環芳香族炭化水素類を抽出した。結果を表4に示
す。
Comparative Example 3 The remaining half of the filter paper obtained in Example 3 was used as a solid sample. It was used without dehydration according to JIS method. The polycyclic aromatic hydrocarbons were extracted with 300 ml of toluene over 16 hours using a Soxhlet extractor. Table 4 shows the results.

【0043】実施例4 ガラス繊維濾紙を付けたハイボリュームエアサンプラー
でディーゼルトラック排ガスを採取し、当該濾紙をそれ
ぞれ2分割し、半分の濾紙を小さく切って固体試料を調
製した。容器(1)に約30mlの固体試料を充填し、
実施例1と同様にしてエタノール及びトルエンを容器
(1)に供給し多環芳香族炭化水素類を抽出した。エタ
ノールの供給量は60ml、トルエンの供給量は150
mlとした。また、トルエンの温度は80℃、空筒線速
度は1cm/分とした(通液時間50分)。結果を表4に
示す。
Example 4 Exhaust gas from a diesel truck was collected with a high-volume air sampler equipped with glass fiber filter paper, the filter paper was divided into two parts, and half of the filter paper was cut into small pieces to prepare a solid sample. Fill container (1) with about 30 ml of solid sample,
In the same manner as in Example 1, ethanol and toluene were supplied to the vessel (1) to extract polycyclic aromatic hydrocarbons. The supply amount of ethanol is 60 ml, and the supply amount of toluene is 150
ml. The temperature of the toluene was 80 ° C., and the linear velocity of the hollow cylinder was 1 cm / min (liquid passing time: 50 minutes). Table 4 shows the results.

【0044】比較例4 実施例4で得た残りの半分の濾紙を固体試料として使用
した。JIS法に従って脱水せずに使用した。ソックス
レー抽出器により、300mlのトルエンで16時間に
亘り多環芳香族炭化水素類を抽出した。結果を表4に示
す。
Comparative Example 4 The remaining half of the filter paper obtained in Example 4 was used as a solid sample. It was used without dehydration according to JIS method. The polycyclic aromatic hydrocarbons were extracted with 300 ml of toluene over 16 hours using a Soxhlet extractor. Table 4 shows the results.

【0045】[0045]

【表4】 [Table 4]

【0046】表4に示す結果から明らかな様に、抽出溶
剤の循環使用を行わない本発明の抽出方法は、抽出溶剤
の循環使用を行うソックスレー抽出法に比し、約10%
抽出量が多く、抽出効果が高い。すなわち、本発明の抽
出方法は、固体試料中の様々な有機物に対して、従来法
より極めて迅速に高い抽出率が得られる。
As is evident from the results shown in Table 4, the extraction method of the present invention in which the extraction solvent is not recycled is about 10% less than the Soxhlet extraction method in which the extraction solvent is recycled.
The extraction amount is large and the extraction effect is high. That is, according to the extraction method of the present invention, a high extraction rate can be obtained for various organic substances in a solid sample much more rapidly than the conventional method.

【0047】[0047]

【発明の効果】以上説明した本発明によれば、固体試料
中の微量目的成分の濃縮回収手段として好適であって、
高い抽出速度が得られる様に改良された簡易な抽出方法
および抽出装置が提供され、本発明の工業的価値は顕著
である。
According to the present invention described above, it is suitable as a means for concentrating and recovering a trace amount of a target component in a solid sample,
A simple extraction method and an extraction apparatus improved so as to obtain a high extraction rate are provided, and the industrial value of the present invention is remarkable.

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

【図1】本発明の好ましい態様の抽出装置の一例の説明
図で
FIG. 1 is a diagram illustrating an example of an extraction device according to a preferred embodiment of the present invention.

【符号の説明】[Explanation of symbols]

1:固体試料充填用容器 11:固体試料 2:容器加熱機構 3:抽出溶剤供給配管 4:定流量ポンプ 5:配管加熱機構 6:抽出液導出配管 6a:抽出溶剤リザーバー 6b:抽出溶剤リザーバー 7:受器 1: Container for solid sample filling 11: Solid sample 2: Container heating mechanism 3: Extraction solvent supply pipe 4: Constant flow pump 5: Pipe heating mechanism 6: Extraction liquid outlet pipe 6a: Extraction solvent reservoir 6b: Extraction solvent reservoir 7: Receiver

Claims (6)

    【特許請求の範囲】[Claims]
  1. 【請求項1】 容器に固体試料を充填し、当該容器の上
    部または下部の一方から抽出溶剤を連続的に通液させて
    固体試料と接触させ、固体試料中の目的成分を抽出して
    当該容器の他方から流出する抽出溶剤を循環せずに回収
    する抽出方法であって、抽出溶剤として沸点が50〜2
    00℃範囲の抽出溶剤を使用し、固体試料に接触する直
    前の抽出溶剤の温度をその沸点より10℃以上低い範囲
    の一定の温度とし、当該容器の上部に存在する抽出溶剤
    の温度が下部に存在する抽出溶剤の温度より10℃以内
    の範囲で高くなる様に固体試料の温度を制御し、抽出溶
    剤の通液速度を0.5〜5cm/分の範囲の一定の空筒
    線流速に制御することを特徴とする抽出方法。
    1. A container is filled with a solid sample, and an extraction solvent is continuously passed through one of the upper and lower portions of the container to make contact with the solid sample to extract a target component in the solid sample. An extraction method wherein the extraction solvent flowing out of the other is recovered without circulation, wherein the extraction solvent has a boiling point of 50 to 2
    Using an extraction solvent in the range of 00 ° C, the temperature of the extraction solvent immediately before coming into contact with the solid sample is set to a constant temperature in a range of at least 10 ° C lower than its boiling point, and the temperature of the extraction solvent present in the upper part of the vessel is lower. The temperature of the solid sample is controlled so as to be higher than the temperature of the existing extraction solvent within 10 ° C., and the flow rate of the extraction solvent is controlled to a constant cylinder linear velocity in the range of 0.5 to 5 cm / min. An extraction method characterized by:
  2. 【請求項2】 抽出溶剤として非親水性抽出溶剤を使用
    する請求項1に記載の抽出方法。
    2. The extraction method according to claim 1, wherein a non-hydrophilic extraction solvent is used as the extraction solvent.
  3. 【請求項3】 親水性溶剤を通液させて固体試料の脱水
    を行なった後に非親水性抽出溶剤を通液させる請求項2
    に記載の抽出方法。
    3. A non-hydrophilic extraction solvent is passed after a hydrophilic solvent is passed through to dehydrate a solid sample.
    Extraction method described in 1.
  4. 【請求項4】 固体試料充填用容器(1)、当該容器の
    周囲に配置された容器加熱機構(2)、抽出溶剤リザー
    バーに連結され且つ容器(1)の上部または下部の一方
    に接続された抽出溶剤供給配管(3)、当該抽出溶剤供
    給配管の少なくとも容器側先端の周囲に配置された配管
    加熱機構(5)、容器(1)の他方に接続された抽出液
    導出配管(6)、固体試料充填用容器(1)に抽出溶剤
    リザーバー中の抽出溶剤を供給する定流量送液機構から
    主として構成されて成ることを特徴とする抽出装置。
    4. A container (1) for filling a solid sample, a container heating mechanism (2) disposed around the container, connected to an extraction solvent reservoir, and connected to one of an upper part and a lower part of the container (1). An extraction solvent supply pipe (3), a pipe heating mechanism (5) disposed at least around the tip of the extraction solvent supply pipe on the container side, an extraction liquid outlet pipe (6) connected to the other of the container (1), a solid An extraction apparatus mainly comprising a constant flow rate liquid feeding mechanism for supplying an extraction solvent in an extraction solvent reservoir to a sample filling container (1).
  5. 【請求項5】 定流量送液機構が抽出溶剤供給配管
    (3)の途中に配置された定流量ポンプ(4)である請
    求項4に記載の抽出装置。
    5. The extraction device according to claim 4, wherein the constant flow rate liquid sending mechanism is a constant flow rate pump (4) arranged in the middle of the extraction solvent supply pipe (3).
  6. 【請求項6】 定流量送液機構が抽出溶剤リザーバーの
    内部にガス圧力を作用させる加圧手段である請求項4に
    記載の抽出装置。
    6. The extraction apparatus according to claim 4, wherein the constant flow rate liquid sending mechanism is a pressurizing means for applying a gas pressure to the inside of the extraction solvent reservoir.
JP2001068053A 2001-03-12 2001-03-12 Extraction method and extraction device Pending JP2002263402A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103298353A (en) * 2010-12-29 2013-09-11 皇家飞利浦电子股份有限公司 Method and apparatus for decocting ingredients in a solvent

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50109287A (en) * 1974-01-31 1975-08-28
JPH02117904A (en) * 1988-10-26 1990-05-02 Asahi Denka Kogyo Kk Extraction
JP2000175823A (en) * 1998-10-09 2000-06-27 Norihisa Kawamura Multifunctional extractor, extraction method using the same and extraction system using the same
JP2000266645A (en) * 1999-03-19 2000-09-29 Kawasaki Steel Corp Extraction method and extracting apparatus for sample containing moisture using organic solvent

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50109287A (en) * 1974-01-31 1975-08-28
JPH02117904A (en) * 1988-10-26 1990-05-02 Asahi Denka Kogyo Kk Extraction
JP2000175823A (en) * 1998-10-09 2000-06-27 Norihisa Kawamura Multifunctional extractor, extraction method using the same and extraction system using the same
JP2000266645A (en) * 1999-03-19 2000-09-29 Kawasaki Steel Corp Extraction method and extracting apparatus for sample containing moisture using organic solvent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103298353A (en) * 2010-12-29 2013-09-11 皇家飞利浦电子股份有限公司 Method and apparatus for decocting ingredients in a solvent

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