JPH05126699A - Purge/trap device - Google Patents
Purge/trap deviceInfo
- Publication number
- JPH05126699A JPH05126699A JP3319715A JP31971591A JPH05126699A JP H05126699 A JPH05126699 A JP H05126699A JP 3319715 A JP3319715 A JP 3319715A JP 31971591 A JP31971591 A JP 31971591A JP H05126699 A JPH05126699 A JP H05126699A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- trap
- chamber
- water
- purge
- 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
Links
- 238000010926 purge Methods 0.000 title abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000007789 gas Substances 0.000 claims abstract description 14
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims description 20
- 239000003463 adsorbent Substances 0.000 claims description 5
- 238000003795 desorption Methods 0.000 claims description 5
- 238000000642 dynamic headspace extraction Methods 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims 1
- 239000000284 extract Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 235000006629 Prosopis spicigera Nutrition 0.000 description 1
- 240000000037 Prosopis spicigera Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、試料から揮発性成分を
抽出し、ガスクロマトグラフに導入するパ―ジアンドト
ラップ装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a page and trap device for extracting a volatile component from a sample and introducing it into a gas chromatograph.
【０００２】[0002]
【従来の技術】パ―ジアンドトラップ装置は、試料から
揮発性成分を連続的に抽出する抽出部と抽出された成分
を吸着剤に捕集するトラップ部から構成されている。ト
ラップ部は抽出された成分を捕集後任意の温度をかけて
加熱脱着し、ガスクロマトグラフに導入する。しかし、
このような装置において固体試料中に含有している水分
を測定する場合、試料表面に吸着している水分も同時に
検出されてしまい試料含有水分のみを分析するのは難し
い。近年では、試料中の水分を完全に除去する目的で、
揮発性成分を捕集および加熱脱着させるトラップ管の前
に、炭酸カルシウム等を充填した水分除去用トラップ管
を設けたパ―ジアンドトラップ装置が用いられたり、氷
−水を用いて０℃に保持した水分除去用トラップ管を設
け、一度水分除去を行った後、目的成分を他のトラップ
管で補集し、加熱脱着する前にそのトラップ管をパ―ジ
して再度水分の除去を行う方法も開発されている。ま
た、他の方法として、コンデンサ―を用いて冷却したト
ラップ管を水分除去用に設ける方法もある。2. Description of the Related Art A page and trap device is composed of an extraction section for continuously extracting volatile components from a sample and a trap section for collecting the extracted components in an adsorbent. The trap portion collects the extracted components, heats and desorbs them at an arbitrary temperature, and introduces them into the gas chromatograph. But,
When measuring the water content contained in a solid sample in such an apparatus, the water content adsorbed on the sample surface is also detected at the same time, and it is difficult to analyze only the sample-containing water content. In recent years, for the purpose of completely removing water in the sample,
A page and trap device provided with a water removal trap tube filled with calcium carbonate or the like before the trap tube for collecting and desorbing volatile components is used, or ice-water is used to raise the temperature to 0 ° C. Provide a trap tube for removing retained water, remove water once, then collect the target component with another trap tube and purge the trap tube before heat desorption to remove moisture again. Methods have also been developed. In addition, as another method, there is a method in which a trap tube cooled by using a condenser is provided for removing water.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、このよ
うなパ―ジアンドトラップ装置では、試料から全ての水
分の除去はできるが、試料表面の吸着水と試料内部の水
を区別し、試料表面吸着水を除去し試料内部水をそのま
ま保持し分析対象とすることができない問題点があっ
た。本発明の目的は、前記問題点を解消し、試料表面吸
着水をパ―ジ除去し、試料含有水分を測定することがで
きるパ―ジアンドトラップ装置を提供することにある。However, although such a purge and trap device can remove all the water from the sample, the water adsorbed on the sample surface can be distinguished from the water adsorbed on the sample surface. There is a problem that water cannot be removed and the water inside the sample cannot be retained as it is for analysis. An object of the present invention is to solve the above problems, to provide a page and trap device capable of purging the water adsorbed on the sample surface and measuring the water content in the sample.
【０００４】[0004]
【課題を解決するための手段】本発明は、試料から揮発
性成分を抽出する抽出部を収納する試料抽出チャンバ
と、抽出した揮発性成分を吸着剤に吸着濃縮した後、加
熱脱着させてガスクロマトグラフに導入するトラップ部
とを有する装置において、試料抽出チャンバの上部に、
該試料を不活性ガスによりガスパ―ジすると共に該試料
の温度コントロ―ルをする予備パ―ジ室を備えることを
特徴とするパ―ジアンドトラップ装置、および試料から
揮発性成分を抽出する抽出部を収納する試料抽出チャン
バと、抽出した揮発性成分を吸着剤に吸着濃縮した後、
加熱脱着させてガスクロマトグラフに導入するトラップ
部とを有する装置において、試料抽出チャンバの上部
に、試料表面吸着水を真空排気すると共に該試料の温度
コントロ―ルをする予備排気室を備えることを特徴とす
るパ―ジアンドトラップ装置である。According to the present invention, a sample extraction chamber for accommodating an extraction unit for extracting a volatile component from a sample and an adsorbent for adsorbing and concentrating the extracted volatile component, followed by heating and desorption for gas chromatography. In a device having a trap part to be introduced into the topography, in the upper part of the sampling chamber,
A purge and trap device, characterized by comprising a preliminary purge chamber for gas-parging the sample with an inert gas and controlling the temperature of the sample, and extraction for extracting volatile components from the sample After the sample extraction chamber that stores the part and the extracted volatile components are adsorbed and concentrated on the adsorbent,
An apparatus having a trap section for heating and desorbing and introducing it into a gas chromatograph, characterized in that a pre-exhaust chamber for vacuum-exhausting the sample surface-adsorbed water and controlling the temperature of the sample is provided above the sample extraction chamber. It is a page and trap device.
【０００５】[0005]
【作用】本発明によれば予備パ―ジ室内で試料に適当な
温度をかけることができると共に不活性ガスにてパ―ジ
することにより試料表面に付着していた水分を完全に除
去することができる。従って、試料表面に吸着水が付着
している如何なる試料においても試料表面に吸着してい
る水分は完全に除去でき、試料内部水は除去されること
なく精度よくパ―ジ・トラップすることができる。また
予備排気室内では、試料に適当な温度をかけることがで
きると共に真空引きすることにより試料表面に付着して
いた水分を完全に除去することができる。従って、試料
表面に吸着水が付着している如何なる試料においても試
料表面に吸着している水分は完全に除去でき、試料内部
水は除去されることなく精度よくパ―ジ・トラップする
ことができる。According to the present invention, the sample can be heated to an appropriate temperature in the preparatory chamber and the moisture adhering to the sample surface can be completely removed by purging with an inert gas. You can Therefore, the water adsorbed on the sample surface can be completely removed from any sample having adsorbed water on the sample surface, and the water inside the sample can be accurately purged and trapped without being removed. .. Further, in the preliminary exhaust chamber, the sample can be heated at an appropriate temperature, and by vacuuming, the water adhering to the sample surface can be completely removed. Therefore, the water adsorbed on the sample surface can be completely removed from any sample having adsorbed water on the sample surface, and the water inside the sample can be accurately purged and trapped without being removed. ..
【０００６】[0006]
【実施例】以下、本発明の一実施例について図面を参照
して詳細に説明する。 実施例１ 図１は本実施例のパ―ジアンドトラップ装置の概略構成
図である。本装置は、予備パ―ジ室１に続く試料抽出チ
ャンバ２および揮発性成分トラップ管３よりなり、予備
パ―ジ室１は試料を加熱するヒ―タ４と、予備パ―ジ室
１と試料抽出チャンバ２との間を遮断するコック５と、
試料をガスパ―ジするパ―ジガス導入管６とを備えてい
る。予備パ―ジ室１には、試料瓶７が装填され、、試料
瓶７にはパ―ジガスの排気口を設けた試料管装着棒８が
備えられている。また試料抽出チャンバ２は、試料を加
熱するヒ―タ９と試料瓶ホルダ１０とキャリヤーガス導
入管１１を備えている。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described in detail below with reference to the drawings. Embodiment 1 FIG. 1 is a schematic configuration diagram of a page and trap device of this embodiment. The apparatus comprises a sample extraction chamber 2 and a volatile component trap tube 3 following a spare page chamber 1. The spare page chamber 1 includes a heater 4 for heating a sample, and a spare page chamber 1. A cock 5 for shutting off the connection with the sample extraction chamber 2,
A purge gas introducing pipe 6 for gas purging the sample is provided. A sample bottle 7 is loaded in the preliminary purge chamber 1, and the sample bottle 7 is provided with a sample tube mounting rod 8 provided with a purge gas exhaust port. The sample extraction chamber 2 also includes a heater 9 for heating the sample, a sample bottle holder 10, and a carrier gas introduction pipe 11.
【０００７】試料は予備パ―ジ室１の試料瓶７中で加熱
およびガスパ―ジされる。パ―ジガスは試料瓶７下部よ
り導入され、試料管装着棒８の排気口より排気される。
これにより試料表面に吸着されていた水分を完全に除去
することができる。試料の十分なパ―ジ後、コック５を
開き、試料抽出チャンバ２の試料瓶ホルダ１０に試料瓶
７を試料管装着棒８により装填し、試料から揮発性成分
を抽出する。抽出された揮発性成分は揮発性成分排出管
１２を通り、揮発性成分トラップ管３に導入され濃縮さ
れる。その後、加熱脱着が行われ、ガスクロマトグラフ
（図示せず。）の試料導入部に導かれる。以上のように
して、試料表面に水分が吸着しているような試料でも試
料表面吸着水を完全に除去し、試料内部に含有している
水分を精度よくパ―ジ・トラップすることができる。The sample is heated and gas paged in the sample bottle 7 of the preparatory chamber 1. The purge gas is introduced from the lower part of the sample bottle 7 and exhausted from the exhaust port of the sample tube mounting rod 8.
As a result, the water adsorbed on the sample surface can be completely removed. After sufficient purging of the sample, the cock 5 is opened, and the sample bottle holder 10 of the sample extraction chamber 2 is loaded with the sample bottle 7 by the sample tube mounting rod 8 to extract volatile components from the sample. The extracted volatile component passes through the volatile component discharge pipe 12, is introduced into the volatile component trap pipe 3, and is concentrated. After that, heat desorption is performed and the sample is introduced to a sample introduction part of a gas chromatograph (not shown). As described above, even in a sample in which water is adsorbed on the sample surface, the water adsorbed on the sample surface can be completely removed, and the water contained in the sample can be precisely trapped.
【０００８】実施例２ 次に、本発明の他の実施例を図面を参照して詳細に説明
する。図２は本実施例を示すパ―ジアンドトラップ装置
の概略構成図である。本装置は、予備排気室２１に続く
試料抽出チャンバ２および揮発性成分トラップ管３より
なり、予備排気室２１は試料を加熱するヒ―タ４と、予
備排気室２１と試料抽出チャンバ２との間を遮断するコ
ック５と、試料を真空引きする真空ポンプ１３と、電磁
弁１４さらに不活性ガス導入管１５と、電磁弁１６を備
えている。予備排気室２１には、試料瓶７が装填され、
試料瓶７には試料管装着棒８が備えられている。また試
料抽出チャンバ２は、試料を加熱するヒ―タ９と、試料
瓶ホルダ１０と、キャリヤーガス導入管１１を備えた構
造である。Embodiment 2 Next, another embodiment of the present invention will be described in detail with reference to the drawings. FIG. 2 is a schematic configuration diagram of the page and trap device according to the present embodiment. This device comprises a sample extraction chamber 2 and a volatile component trap tube 3 following a preliminary exhaust chamber 21, and the preliminary exhaust chamber 21 includes a heater 4 for heating a sample, a preliminary exhaust chamber 21 and a sample extraction chamber 2. A cock 5 for shutting off the space, a vacuum pump 13 for evacuating the sample, a solenoid valve 14, an inert gas introducing pipe 15, and a solenoid valve 16 are provided. The pre-evacuation chamber 21 is loaded with the sample bottle 7,
The sample bottle 7 is equipped with a sample tube mounting rod 8. The sample extraction chamber 2 has a structure including a heater 9 for heating a sample, a sample bottle holder 10, and a carrier gas introduction pipe 11.
【０００９】試料は予備排気室２１の試料瓶７中で加熱
し、真空ポンプ１３より電磁弁１４を開き試料表面吸着
水を排気する。これにより試料表面に吸着されていた水
分を完全に除去することができる。試料表面の吸着水を
除去後、電磁弁１４を閉じ、電磁弁１６を開くことによ
り不活性ガス導入管１５より不活性ガスを導入する。そ
の後、コック５を開き試料抽出チャンバ２の試料瓶ホル
ダ１０に試料瓶７を試料管装着棒８により装填し、試料
から揮発性成分を抽出する。抽出された揮発性成分は揮
発性成分排出管１２を通り揮発性成分トラップ管３に導
入され濃縮される。その後、加熱脱着が行われ、ガスク
ロマトグラフの試料導入部に導かれる。以上のようにし
て、試料表面に水分が吸着しているような試料でも試料
表面吸着水を完全に除去し、試料内部に含有している水
分を精度よくパ―ジ・トラップすることができる。The sample is heated in the sample bottle 7 in the preliminary exhaust chamber 21, and the electromagnetic valve 14 is opened by the vacuum pump 13 to exhaust the water adsorbed on the sample surface. As a result, the water adsorbed on the sample surface can be completely removed. After removing the adsorbed water on the surface of the sample, the electromagnetic valve 14 is closed and the electromagnetic valve 16 is opened to introduce the inert gas from the inert gas introducing pipe 15. Then, the cock 5 is opened and the sample bottle holder 10 of the sample extraction chamber 2 is loaded with the sample bottle 7 by the sample tube mounting rod 8 to extract volatile components from the sample. The extracted volatile component is introduced into the volatile component trap pipe 3 through the volatile component discharge pipe 12 and concentrated. After that, thermal desorption is performed and the sample is introduced to the sample introduction section of the gas chromatograph. As described above, even in a sample in which water is adsorbed on the sample surface, the water adsorbed on the sample surface can be completely removed, and the water contained in the sample can be precisely trapped.
【００１０】[0010]
【発明の効果】以上説明したように、本発明によるパ―
ジアンドトラップ装置を用いることにより、試料表面に
吸着水が付着されていても吸着水を完全に除去し、試料
内部に含有している水分を精度よくパ―ジ・トラップす
ることが可能となる。As described above, the part according to the present invention is used.
By using the Jand trap device, even if adsorbed water is attached to the sample surface, it is possible to completely remove the adsorbed water and to accurately purge and trap the water content inside the sample. ..
【図１】本発明の一実施例の概略構成図である。FIG. 1 is a schematic configuration diagram of an embodiment of the present invention.
【図２】本発明の他の一実施例の概略構成図である。FIG. 2 is a schematic configuration diagram of another embodiment of the present invention.
１ 予備パ―ジ室 ２ 試料抽出チャンバ ３ 揮発性成分トラップ管 ４ ヒ―タ ５ コック ６ パ―ジガス導入管 ７ 試料瓶 ８ 試料管装着棒 ９ ヒ―タ １０ 試料瓶ホルダ １１ キャリヤーガス導入管 １２ 揮発性成分排出
管 １３ 真空ポンプ １４，１６ 電磁弁 １５ 不活性ガス導入管 ２１ 予備排気室1 Spare Purging Chamber 2 Sample Extraction Chamber 3 Volatile Component Trap Tube 4 Heater 5 Cock 6 Purging Gas Introducing Tube 7 Sample Bottle 8 Sample Tube Mounting Rod 9 Heater 10 Sample Bottle Holder 11 Carrier Gas Introducing Tube 12 Volatile component discharge pipe 13 Vacuum pump 14,16 Solenoid valve 15 Inert gas introduction pipe 21 Preliminary exhaust chamber
Claims (2)
収納する試料抽出チャンバと、抽出した揮発性成分を吸
着剤に吸着濃縮した後、加熱脱着させてガスクロマトグ
ラフに導入するトラップ部とを有する装置において、試
料抽出チャンバの上部に、該試料を不活性ガスによりガ
スパ―ジすると共に該試料の温度コントロ―ルをする予
備パ―ジ室を備えることを特徴とするパ―ジアンドトラ
ップ装置。1. A sample extraction chamber containing an extraction unit for extracting volatile components from a sample, and a trap unit for adsorbing and concentrating the extracted volatile components on an adsorbent, followed by heat desorption and introduction into a gas chromatograph. In the apparatus having the above, the purge and trap apparatus is characterized in that, in the upper part of the sample extraction chamber, there is provided a preparatory chamber for gas-perging the sample with an inert gas and controlling the temperature of the sample. ..
収納する試料抽出チャンバと、抽出した揮発性成分を吸
着剤に吸着濃縮した後、加熱脱着させてガスクロマトグ
ラフに導入するトラップ部とを有する装置において、試
料抽出チャンバの上部に、試料表面吸着水を真空排気す
ると共に該試料の温度コントロ―ルをする予備排気室を
備えることを特徴とするパ―ジアンドトラップ装置。2. A sample extraction chamber that houses an extraction unit that extracts volatile components from a sample, and a trap unit that adsorbs and concentrates the extracted volatile components on an adsorbent, then heat-desorbs them and introduces them into a gas chromatograph. The page and trap device, wherein the apparatus has a pre-exhaust chamber for vacuum-exhausting the sample surface adsorbed water and for controlling the temperature of the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3319715A JPH05126699A (en) | 1991-11-08 | 1991-11-08 | Purge/trap device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3319715A JPH05126699A (en) | 1991-11-08 | 1991-11-08 | Purge/trap device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05126699A true JPH05126699A (en) | 1993-05-21 |
Family
ID=18113371
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3319715A Pending JPH05126699A (en) | 1991-11-08 | 1991-11-08 | Purge/trap device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05126699A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2023538307A (en) * | 2020-08-11 | 2023-09-07 | エンテック インスツルメンツ インコーポレイテッド | Systems and methods for matrix-accelerated vacuum-assisted sorbent extraction to improve sample preparation prior to GCMS analysis |
| US12158454B2 (en) | 2018-07-31 | 2024-12-03 | Entech Instruments Inc. | Hybrid capillary/packed trap and method of use |
-
1991
- 1991-11-08 JP JP3319715A patent/JPH05126699A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12158454B2 (en) | 2018-07-31 | 2024-12-03 | Entech Instruments Inc. | Hybrid capillary/packed trap and method of use |
| JP2023538307A (en) * | 2020-08-11 | 2023-09-07 | エンテック インスツルメンツ インコーポレイテッド | Systems and methods for matrix-accelerated vacuum-assisted sorbent extraction to improve sample preparation prior to GCMS analysis |
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