JPH08160024A - Collection and analysis of very small amount of volatile component in solution - Google Patents
Collection and analysis of very small amount of volatile component in solutionInfo
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- JPH08160024A JPH08160024A JP30594494A JP30594494A JPH08160024A JP H08160024 A JPH08160024 A JP H08160024A JP 30594494 A JP30594494 A JP 30594494A JP 30594494 A JP30594494 A JP 30594494A JP H08160024 A JPH08160024 A JP H08160024A
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- volatile component
- component
- solution
- cooled
- soln
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、水、有機溶媒等の溶液
中に拡散溶解している微量の揮発性成分を捕集する方法
と捕集した微量揮発性成分を分析する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for collecting a trace amount of volatile components diffused and dissolved in a solution such as water or an organic solvent, and a method for analyzing the collected trace volatile components.
【０００２】[0002]
【従来の技術】従来より水、有機溶媒等溶液中に存在し
ている低沸点の揮発性成分を捕集して、定量、定性分析
する方法として、ガラス製等の密封可能な容器内にこの
液体を入れ、外部から加熱し、容器内のヘッドスペース
に放たれる物質を注射器等で抜き取り、ガスクロマトグ
ラフィーで分析する方法がある。しかし、この方法は加
熱により、測定対象成分が分解してしまう可能性があ
り、また、溶媒が大量に存在するため精度良く分析する
ことができないという問題がある。2. Description of the Related Art Conventionally, as a method for collecting, quantitatively and qualitatively analyzing low-boiling volatile components existing in a solution such as water or an organic solvent, the method has been conducted in a sealable container such as glass. There is a method in which a liquid is put in, heated from the outside, the substance released to the head space in the container is extracted with a syringe or the like, and analyzed by gas chromatography. However, this method has a problem in that the component to be measured may be decomposed by heating and the solvent cannot be analyzed accurately because of the large amount of solvent.
【０００３】また、加熱せずに溶液中にアルゴンガス、
ヘリウムガスのような不活性ガスをバブリングさせて、
溶液を飽和させることで、追い出される揮発性成分を捕
らえて、それをガスクロマトグラフィーで分析する方法
もあるが、この方法では追い出される揮発性成分が極微
量であるため、定量、定性分析ができない場合もある。Argon gas in the solution without heating,
Bubble an inert gas such as helium gas,
By saturating the solution, there is also a method to capture the volatile components that are expelled and analyze it by gas chromatography, but this method does not allow quantitative and qualitative analysis because the volatile components that are expelled are extremely small. In some cases.
【０００４】[0004]
【発明が解決しようとする課題】そこで本発明は、溶液
中に存在している微量の揮発性成分を捕集して、分析す
る方法に関する上記のような問題点を除去するためにな
されたもので、溶液中に存在している揮発性成分を、当
該成分が分解してしまうような加熱をすることなく効率
良く捕集して、精度良く分析する方法を提供することを
目的とする。Therefore, the present invention has been made to eliminate the above-mentioned problems relating to a method for collecting and analyzing a trace amount of volatile components present in a solution. Then, it is an object of the present invention to provide a method for efficiently collecting volatile components existing in a solution without heating such that the components are decomposed and analyzing them with high accuracy.
【０００５】[0005]
【課題を解決するための手段】本発明は上記目的を達成
するために、まず第１の発明では、溶液中の微量揮発性
成分を捕集する方法であって、溶液を低温度で冷却固化
し、この冷却固化した物質を高真空状態で減圧乾燥し、
その際気化する揮発性成分を、捕集剤に吸着させて捕集
することを特徴とする溶液中の微量揮発性成分の捕集方
法を提供するものである。In order to achieve the above-mentioned object, the present invention is, in the first invention, a method for collecting a trace amount of volatile components in a solution, wherein the solution is cooled and solidified at a low temperature. Then, this cooled and solidified material is dried under reduced pressure in a high vacuum state,
The present invention provides a method for collecting a trace amount of a volatile component in a solution, which is characterized in that a volatile component vaporized at that time is adsorbed by a scavenger to be collected.
【０００６】また、第２の発明では、第１の発明の方法
により捕集した微量揮発性成分を、捕集剤を加温しなが
ら不活性ガスで置換することにより捕集剤から追い出
し、追い出した揮発性成分を低温度でトラップし、トラ
ップした成分をガスクロマトグラフィーにより分析する
ことを特徴とする捕集した微量揮発性成分の分析方法を
提供するものである。In the second invention, the trace volatile components collected by the method of the first invention are displaced from the scavenger by replacing the scavenger with an inert gas while heating the scavenger. Another object of the present invention is to provide a method for analyzing a collected trace volatile component, which comprises trapping the volatile component at a low temperature and analyzing the trapped component by gas chromatography.
【０００７】[0007]
【作用】上記のように本発明によれば、溶液を低温度で
冷却固化し、この冷却固化した物質を真空状態で減圧乾
燥し、その際発生する揮発性成分を捕集剤を介して捕集
するので、加熱操作を必要とせず、測定対象成分が熱分
解することがない。また、捕集剤に吸着された揮発性成
分を捕集剤から分離する際にも、当該成分が分解するよ
うな加熱操作をせずに分離するので、測定対象成分が熱
分解することがない。As described above, according to the present invention, the solution is cooled and solidified at a low temperature, the cooled and solidified material is dried under reduced pressure in a vacuum, and the volatile components generated at that time are collected through a collector. Since they are collected, the heating operation is not required and the components to be measured are not thermally decomposed. Further, even when the volatile component adsorbed to the scavenger is separated from the scavenger without performing a heating operation such that the component is decomposed, the measurement target component is not thermally decomposed. .
【０００８】[0008]
【実施例】以下実施例により本発明を詳細に説明する。
図１は、本発明による溶液中の微量揮発性成分の捕集方
法と、捕集した微量揮発性成分の分析方法に関する工程
説明図である。The present invention will be described in detail with reference to the following examples.
FIG. 1 is a process explanatory diagram relating to a method for collecting a trace volatile component in a solution and an analysis method for a collected trace volatile component according to the present invention.
【０００９】測定対象成分である揮発性成分の溶けてい
る試料溶液（１０）を、凍結乾燥機にセット（１１）
し、−５０°Ｃで０，５時間運転し、対象試料溶液を冷
却、固化（１２）させる。ついで、この冷却、固化した
対象試料物を、０，０３ｍｍＨｇの高真空下で減圧、乾
燥（１３）する。その際、対象試料溶液中に溶けている
測定対象成分である有機物等の揮発性成分は気化（１
４）するので、その揮発性成分を捕捉する捕捉部（減圧
手段と試料収容部をつなぐ通路上に配置される）に、揮
発性成分を吸着等して捕らえる捕集剤を装備しておく。A sample solution (10) in which a volatile component to be measured is dissolved is set in a freeze dryer (11).
Then, the target sample solution is cooled and solidified (12) by operating at −50 ° C. for 0.5 hours. Then, the cooled and solidified target sample is decompressed and dried (13) under a high vacuum of 0.03 mmHg. At that time, a volatile component such as an organic substance which is a measurement target component dissolved in the target sample solution is vaporized (1
4) Therefore, the trapping portion (disposed on the passage connecting the decompression means and the sample storage portion) for trapping the volatile component is equipped with a scavenger for adsorbing the volatile component.
【００１０】ここで、試料溶液を固化させるのは、液体
状態のままで減圧すると突沸現象を起こす可能性が高
く、そのまま気化せずに液体状態のまま飛び出してしま
うのを防ぐ意味からである。また、冷却、固化すると、
それが一定温度下で減圧状態を保つことができるからで
ある。Here, the reason why the sample solution is solidified is that there is a high possibility that a bumping phenomenon will occur if the pressure is reduced in the liquid state, and that the sample solution does not vaporize as it is and jumps out in the liquid state. Also, when cooled and solidified,
This is because it can maintain a reduced pressure at a constant temperature.
【００１１】捕集剤としては、表面積の大きいグラファ
イトカーボン、合成ゼオライト（モレキュラーシーブ
ス）、スチレン・ジビニルベンゼン共重合体（直鎖型、
架橋型）、ポリビニルピロリドン、ポリビニルピリジ
ン、ポリ２，６−ジフェニル−ｐ−フェニレンオキシド
等が使用でき、測定対象物に合わせて適宜、選択又は、
組み合わせて使用する。As the scavenger, graphite carbon having a large surface area, synthetic zeolite (molecular sieves), styrene / divinylbenzene copolymer (straight chain type,
(Crosslinked type), polyvinylpyrrolidone, polyvinylpyridine, poly2,6-diphenyl-p-phenylene oxide, etc. can be used, and selected or selected appropriately according to the measurement object.
Used in combination.
【００１２】試料溶液は減圧下のため、飛散し無くなっ
て行くが、その際、揮発性成分のみは、前記の捕捉部で
捕集剤に吸着（１５）されて濃縮される。The sample solution does not scatter because it is under reduced pressure, but at that time, only the volatile component is adsorbed (15) to the scavenger in the trapping section and concentrated.
【００１３】揮発性成分が吸着された捕集剤を、捕捉部
から取り出し、密閉容器に移し、５０〜６０°Ｃに加温
しながらアルゴンガス、ヘリウムガス、窒素ガス等の不
活性ガスで置換（１６）しながら低温でトラップを行
い、揮発性成分を分離（１７）し、この分離した揮発性
成分のみをガスクロマトグラフィーで分析（１８）する
ことにより捕集物質の定性、定量が可能となる。The scavenger in which the volatile components have been adsorbed is taken out from the trapping section, transferred to a closed container, and replaced with an inert gas such as argon gas, helium gas or nitrogen gas while heating at 50 to 60 ° C. (16) While trapping at a low temperature, the volatile components are separated (17), and the separated volatile components are analyzed (18) by gas chromatography to enable qualitative and quantitative determination of the collected substances. Become.
【００１４】[0014]
【発明の効果】上記のように本発明によれば、目的とす
る成分が分解してしまうような加熱操作を必要とせず、
従って測定対象成分が熱分解しないので、揮発性成分の
正確な定量、定性分析が可能となる。また、水、有機溶
媒等の中に存在する微量の揮発性成分を精度良く分析で
きるので、例えば水質汚染物質の定量、定性分析あるい
は液体食品中に含まれる異味、異臭成分等も捕らえて分
析することが可能となる。As described above, according to the present invention, there is no need for a heating operation that decomposes a target component,
Therefore, since the component to be measured is not thermally decomposed, accurate quantification and qualitative analysis of the volatile component are possible. In addition, since trace amounts of volatile components present in water, organic solvents, etc. can be accurately analyzed, for example, quantitative and qualitative analysis of water pollutants or offensive taste and offensive odor components contained in liquid foods can also be analyzed. It becomes possible.
【図１】本発明の一実施例を示す工程説明図である。FIG. 1 is a process explanatory view showing an embodiment of the present invention.
１０‥‥試料溶液 １１‥‥凍結乾燥機にセット １２‥‥冷却、固化 １３‥‥減圧、乾燥 １４‥‥揮発性成分気化 １５‥‥捕集剤に吸着 １６‥‥不活性ガス置換 １７‥‥揮発性成分分離 １８‥‥ガスクロマトグラフィー分析 10 ... Sample solution 11 ... Set in freeze dryer 12 ... Cooling, solidification 13 ... Decompression, drying 14 ... Volatile component vaporization 15 ... Adsorption to scavenger 16 ... Inert gas replacement 17 ... Separation of volatile components 18 Gas chromatography analysis
Claims (2)
あって、 溶液を低温度で冷却固化し、この冷却固化した物質を高
真空状態で減圧乾燥し、 その際気化する揮発性成分を、捕集剤に吸着させて捕集
することを特徴とする溶液中の微量揮発性成分の捕集方
法。1. A method for collecting a trace volatile component in a solution, which comprises cooling and solidifying the solution at a low temperature, drying this cooled and solidified substance under reduced pressure in a high vacuum state, and vaporizing at that time. A method for collecting a trace amount of a volatile component in a solution, which comprises adsorbing a component onto a scavenger to collect the component.
発性成分を、捕集剤を加温しながら不活性ガスで置換す
ることにより捕集剤から追い出し、 追い出した揮発性成分を低温度でトラップし、 トラップした成分をガスクロマトグラフィーにより分析
することを特徴とする捕集した微量揮発性成分の分析方
法。2. A trace volatile component collected by the method according to claim 1 is displaced from the scavenger by replacing the volatile component with an inert gas while heating the scavenger, and the volatile component displaced is reduced. A method for analyzing a collected trace volatile component, which comprises trapping at a temperature and analyzing the trapped component by gas chromatography.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30594494A JP3404937B2 (en) | 1994-12-09 | 1994-12-09 | Method for collecting trace volatile components in solution and method for analyzing volatile components |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30594494A JP3404937B2 (en) | 1994-12-09 | 1994-12-09 | Method for collecting trace volatile components in solution and method for analyzing volatile components |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08160024A true JPH08160024A (en) | 1996-06-21 |
| JP3404937B2 JP3404937B2 (en) | 2003-05-12 |
Family
ID=17951183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30594494A Expired - Fee Related JP3404937B2 (en) | 1994-12-09 | 1994-12-09 | Method for collecting trace volatile components in solution and method for analyzing volatile components |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3404937B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020193982A (en) * | 2016-03-08 | 2020-12-03 | エンテック インスツルメンツ インコーポレイテッド | Vacuum-assisted sample extraction device and method |
| US11896366B2 (en) | 2018-03-06 | 2024-02-13 | Entech Instruments Inc. | Ventilator-coupled sampling device and method |
-
1994
- 1994-12-09 JP JP30594494A patent/JP3404937B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020193982A (en) * | 2016-03-08 | 2020-12-03 | エンテック インスツルメンツ インコーポレイテッド | Vacuum-assisted sample extraction device and method |
| US11896366B2 (en) | 2018-03-06 | 2024-02-13 | Entech Instruments Inc. | Ventilator-coupled sampling device and method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3404937B2 (en) | 2003-05-12 |
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