JP2010096665A - Sample gas collector and gas chromatograph device - Google Patents

Sample gas collector and gas chromatograph device Download PDF

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JP2010096665A
JP2010096665A JP2008268715A JP2008268715A JP2010096665A JP 2010096665 A JP2010096665 A JP 2010096665A JP 2008268715 A JP2008268715 A JP 2008268715A JP 2008268715 A JP2008268715 A JP 2008268715A JP 2010096665 A JP2010096665 A JP 2010096665A
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sample gas
hollow member
gas
collecting
pipe
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Takahiro Shoda
隆博 荘田
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Yazaki Corp
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Yazaki Corp
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<P>PROBLEM TO BE SOLVED: To contribute improvement of concentration efficiency by a collecting means obtaining a negative pressure effect with a little purge gas when desorbed. <P>SOLUTION: In a sample gas collector 10 when a sample gas flows in the collecting means 11 the collecting means 11 collects the sample gas. The sample gas collector 10 shuts off an upstream side valve 14a, heats the collecting means 11 by a heating means 12, and shuts off a down stream side valve 14b and cools a hollow member 13 by a cooling means 15. The sample gas collector 10 desorbes the sample gas collected in the collecting means 11 into the hollow member 13 instantaneously by opening the upstream side valve 14a. The sample gas collector 10 opens the downstream side valve 14b and discharges the concentration gas desorbed in the hollow member 13 to the downstream of the hollow member 13 by a discharging means 17. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、導入された試料ガスを低温状態のときに捕集し且つ前記捕集した試料ガスを高温状態のときに脱離する捕集部材を有する試料ガス捕集装置及びガスクロマトグラフ装置に関するものである。   The present invention relates to a sample gas collecting apparatus and a gas chromatograph apparatus having a collecting member that collects an introduced sample gas at a low temperature and desorbs the collected sample gas at a high temperature. It is.

ガスクロマトグラフ装置（以下、ＧＣ装置）は、例えば、大気等の試料ガスに含まれる揮発性有機化合物等の検出対象成分の検出に用いられる装置であり、該試料ガスに含まれる微量な成分の検出を可能とするため、分離カラムおよび検出センサなどの検出装置のほかに、検出対象成分を捕集して濃縮するための捕集装置を備えた構成のものが一般的に用いられている。   A gas chromatograph apparatus (hereinafter referred to as a GC apparatus) is an apparatus used for detecting a component to be detected such as a volatile organic compound contained in a sample gas such as the atmosphere, and detects a trace amount component contained in the sample gas. Therefore, in addition to a detection device such as a separation column and a detection sensor, a configuration including a collection device for collecting and concentrating a detection target component is generally used.

特許文献１で提案されているＧＣ装置１００は、図１１に示されるように、試料ガス成分を搬送するキャリアガスを発生するガスボンベなどのキャリアガス源１０８、キャリアガスによって搬送された試料ガスの成分を検出（分析）する分析装置１１０、試料ガスを導入する試料導入口１０１、試料導入口１０１から導入された試料ガスを吸引して排出口１１５から排出する吸引ポンプ１０４、試料ガスから検出対象成分を捕集して濃縮する捕集管１０２、および、捕集管１０２を試料導入口１０１と吸引ポンプ１０４との間またはキャリアガス源１０８と分析装置１１０との間に選択的に接続するバルブ１０５、などから構成されている。   As shown in FIG. 11, the GC apparatus 100 proposed in Patent Document 1 includes a carrier gas source 108 such as a gas cylinder that generates a carrier gas for transporting a sample gas component, and a component of the sample gas transported by the carrier gas. , A sample introduction port 101 for introducing a sample gas, a suction pump 104 for sucking the sample gas introduced from the sample introduction port 101 and discharging it from the discharge port 115, and a component to be detected from the sample gas And a valve 105 for selectively connecting the collection tube 102 between the sample inlet 101 and the suction pump 104 or between the carrier gas source 108 and the analyzer 110. , Etc.

このＧＣ装置１００において、検出対象成分を捕集（濃縮）するときは、捕集管１０２が試料導入口１０１と吸引ポンプ１０４との間に直列に接続されるようバルブ１０５を切り替え、吸引ポンプ１０４が試料ガスを吸引することにより、試料導入口１０１に導入された試料ガスが捕集管１０２内を流動されて検出対象成分が捕集される。   In the GC apparatus 100, when collecting (concentrating) the detection target component, the valve 105 is switched so that the collection tube 102 is connected in series between the sample introduction port 101 and the suction pump 104, and the suction pump 104 is collected. As the sample gas is sucked, the sample gas introduced into the sample introduction port 101 flows in the collection tube 102 and the detection target component is collected.

そして、検出対象成分を検出するときは、冷却加熱装置１１１により捕集管１０２を加熱することで、捕集した試料成分の脱離を促し、捕集管１０２がキャリアガス源１０８と分析装置１１０との間に直列に接続されるようバルブ１０５を切り替えて、キャリアガス源１０８がキャリアガスを発生して捕集管１０２内を流動させることにより、検出対象成分をキャリアガスによって捕集管１０２から分析装置１１０まで搬送して、分析装置１１０内に導入していた。   When detecting the detection target component, the collection tube 102 is heated by the cooling and heating device 111 to promote desorption of the collected sample component, and the collection tube 102 serves as the carrier gas source 108 and the analysis device 110. The carrier gas source 108 generates a carrier gas and flows in the collection tube 102 by switching the valve 105 so as to be connected in series between the detection target component and the carrier gas from the collection tube 102. The sample was transported to the analyzer 110 and introduced into the analyzer 110.

また、ＧＣ装置１００では、捕集管１０２の前記パージガスの流入側流路中にオリフィス１１３を設けたことにより、加熱脱離時に捕集管１０２内でパージガスの流速がオリフィス１１３に絞られて増加し、ベルヌーイ効果により圧力を降下させることで、捕集管１０２からの試料成分の脱離効果を向上させてきた。
特開２００６−３３７１５８号公報 Further, in the GC apparatus 100, the orifice 113 is provided in the purge gas inflow channel of the collection tube 102, so that the flow rate of the purge gas is increased by the orifice 113 in the collection tube 102 during heating and desorption. However, the desorption effect of the sample components from the collection tube 102 has been improved by lowering the pressure by the Bernoulli effect.
JP 2006-337158 A

しかしながら、捕集管の捕集剤から試料成分を脱離させる脱離効果を向上させるには、捕集管内を高温かつ低圧力にすることが好ましいが、実際に捕集管内に負圧を得る（低圧力にする）には、捕集管に大量のパージガスを流す必要があった。ところが、パージガスが多いと、試料ガス、試料成分等が薄まってしまい、分離性が悪くなり、十分な脱離効果を得ることができなかった。また、従来のＧＣ装置ではパージガスも多く必要なため、ガス成分の分析に要するランニングコストを低減させるのが困難であった。   However, in order to improve the desorption effect of desorbing the sample components from the collecting agent of the collecting tube, it is preferable to set the inside of the collecting tube to a high temperature and a low pressure, but actually a negative pressure is obtained in the collecting tube. In order to reduce the pressure, it was necessary to flow a large amount of purge gas through the collection tube. However, when the purge gas is large, the sample gas, sample components and the like are diluted, so that the separability is deteriorated and a sufficient desorption effect cannot be obtained. In addition, since the conventional GC apparatus requires a large amount of purge gas, it is difficult to reduce the running cost required for analyzing the gas components.

よって本発明は、上述した問題点に鑑み、脱離時に少量のパージガスで捕集手段に負圧効果を得て濃縮効率の向上に貢献することができる試料ガス捕集装置及びガスクロマトグラフ装置を提供することを課題としている。   Therefore, in view of the above-described problems, the present invention provides a sample gas collecting device and a gas chromatograph device that can contribute to improving the concentration efficiency by obtaining a negative pressure effect in the collecting means with a small amount of purge gas at the time of desorption. The challenge is to do.

上記課題を解決するため本発明によりなされた請求項１記載の試料ガス捕集装置は、配管に設けられて前記配管内を流れる試料ガスを捕集する捕集手段と、前記捕集手段に捕集した試料ガスが脱離する高温状態に前記捕集手段を加熱する加熱手段と、を有する試料ガス捕集装置において、前記試料ガスの流れ方向の前記配管における前記捕集手段の下流側に設けられた中空状部材と、前記中空状部材を前記捕集手段からの気体の流通が不可能な閉塞状態とその流通が可能な開放状態に切り替える切り替え手段と、前記中空状部材が閉塞状態のときに前記中空状部材を冷却する冷却手段と、前記試料ガスを捕集した捕集手段を前記加熱手段に加熱させ且つ前記中空状部材を前記冷却手段に冷却させる第１制御手段と、前記第１制御手段が前記捕集手段を加熱させ且つ前記中空状部材を冷却させた後に、前記中空状部材を開放状態へ前記切り替え手段に切り替えさせる第２制御手段と、前記第２制御手段による制御に応じて前記捕集手段から脱離した濃縮ガスを排出させる排出手段と、を有することを特徴とする。   In order to solve the above-mentioned problems, a sample gas collecting device according to claim 1 made according to the present invention is provided with a collecting means for collecting a sample gas provided in a pipe and flowing in the pipe, and the collecting means for collecting the sample gas. And a heating means for heating the collecting means to a high temperature state where the collected sample gas is desorbed, provided on the downstream side of the collecting means in the pipe in the flow direction of the sample gas. When the hollow member is in a closed state, and a switching means for switching the hollow member between a closed state in which gas cannot be circulated from the collecting means and an open state in which the flow is possible. Cooling means for cooling the hollow member, first control means for causing the heating means to heat the collecting means for collecting the sample gas, and cooling the hollow member to the cooling means, and the first The control means After the means is heated and the hollow member is cooled, second control means for switching the hollow member to the switching means to the open state, and from the collecting means according to the control by the second control means And a discharge means for discharging the desorbed concentrated gas.

請求項２記載の発明は、請求項１に記載の試料ガス捕集装置において、前記切り替え手段が、前記捕集手段の上流側の前記配管に設けられた上流側弁と、前記中空状部材の下流側の前記配管に設けられた下流側弁と、を有することを特徴とする。   The invention according to claim 2 is the sample gas collecting apparatus according to claim 1, wherein the switching means includes an upstream valve provided in the pipe on the upstream side of the collecting means, and the hollow member. And a downstream valve provided in the pipe on the downstream side.

上記課題を解決するため本発明によりなされた請求項３記載のガスクロマトグラフ装置は、請求項１又は２に記載の試料ガス捕集装置と、前記試料ガス捕集装置で脱離した試料ガスの成分を分析する分析手段と、を有することを特徴とする。   The gas chromatograph apparatus according to claim 3, which has been made according to the present invention to solve the above-mentioned problems, comprises the sample gas collector according to claim 1 or 2 and the components of the sample gas desorbed by the sample gas collector. And analyzing means for analyzing.

以上説明したように請求項１に記載した本発明の試料ガス捕集装置によれば、捕集手段の下流に中空状部材を設け、試料ガスを捕集した捕集手段を加熱し、中空状部材を冷却した後に、捕集手段と中空状部材を流通させるように切り替えることから、高温状態の捕集手段内は一気に低圧力に変化するため、捕集手段に有効な負圧効果を得ることが可能となり、捕集手段から試料ガスを極短時間で脱離させることができる。従って、その脱離した濃縮ガスを排出するのに必要なキャリアガスが少量で良いため、試料ガスの分離性を低下させることなく、十分な脱離効果を得ることができる。   As described above, according to the sample gas collecting device of the present invention described in claim 1, a hollow member is provided downstream of the collecting means, and the collecting means for collecting the sample gas is heated to form a hollow shape. After the member is cooled, the collecting means and the hollow member are switched to flow, so the inside of the collecting means in a high temperature state is changed to a low pressure at a stretch, so that a negative pressure effect effective for the collecting means is obtained. Thus, the sample gas can be desorbed from the collecting means in a very short time. Therefore, since a small amount of carrier gas is required to discharge the desorbed concentrated gas, a sufficient desorption effect can be obtained without degrading the sample gas separation.

請求項２に記載の発明によれば、請求項１に記載の発明の効果に加え、捕集手段の上流側に上流側弁を設けるようにしたことから、捕集手段を中空状部材と共に減圧させることができるため、捕集手段から試料ガスをより一層短時間で脱離させることができる。   According to the invention described in claim 2, in addition to the effect of the invention described in claim 1, since the upstream valve is provided on the upstream side of the collecting means, the collecting means is decompressed together with the hollow member. Therefore, the sample gas can be desorbed from the collecting means in a shorter time.

以上説明したように請求項３に記載した本発明のガスクロマトグラフ装置によれば、捕集した試料ガスの分離性を向上させ且つ短時間で高濃度の試料ガスを送出する試料ガス捕集装置を有していることから、試料ガス捕集装置は分析手段に短時間で高濃度の試料ガスを送出することができ、分析手段は急激な検出ピークを得ることができるため、ガスの成分を効率的に分析することができる。従って、高精度で再現性の良い測定が可能となり、試料ガスの分析に要するランニングコストを削減することができる。   As described above, according to the gas chromatograph apparatus of the present invention described in claim 3, the sample gas collecting apparatus that improves the separability of the collected sample gas and delivers a high concentration sample gas in a short time. Therefore, the sample gas collection device can send a high concentration of sample gas to the analysis means in a short time, and the analysis means can obtain a sudden detection peak. Analysis. Therefore, measurement with high accuracy and good reproducibility is possible, and the running cost required for analyzing the sample gas can be reduced.

以下、本発明に係る試料ガス捕集装置および該試料ガス捕集装置を有するガスクロマトグラフ（ＧＣ）装置の一実施形態について、図１乃至図１０の図面を参照して説明する。   Hereinafter, an embodiment of a sample gas collection device and a gas chromatograph (GC) device having the sample gas collection device according to the present invention will be described with reference to the drawings of FIGS.

図１において、試料ガス捕集装置１０は、捕集手段１１と、加熱手段１２と、中空状部材１３と、切り替え手段１４と、冷却手段１５と、第１制御手段１６ａと、第２制御手段１６ｂと、排出手段１７と、を有して構成している。   In FIG. 1, a sample gas collecting apparatus 10 includes a collecting means 11, a heating means 12, a hollow member 13, a switching means 14, a cooling means 15, a first control means 16a, and a second control means. 16b and discharge means 17 are provided.

捕集手段１１は、配管１０ａに設けられて、その配管１０ａ内を流れる試料ガスを捕集する。捕集手段１１は、図示しないが、例えば、ＴＥＮＡＸ系、活性炭系、ゼオライト系等の、試料ガスを捕集する捕集剤と、この捕集剤を収容する中空筒状の収容部材と、を有している。   The collection means 11 is provided in the pipe 10a and collects the sample gas flowing through the pipe 10a. Although not shown, the collection means 11 includes, for example, a collection agent that collects a sample gas, such as a TENAX system, an activated carbon system, and a zeolite system, and a hollow cylindrical housing member that houses the collection agent. Have.

加熱手段１２は、第１制御手段１６ａと電気的に接続されており、公知であるヒータ等の加熱装置が用いられる。加熱手段１２は、その第１制御手段１６ａ等の制御に応じて、捕集手段１１に捕集した試料ガスが脱離する高温状態に捕集手段１１を加熱する。   The heating means 12 is electrically connected to the first control means 16a, and a known heating device such as a heater is used. The heating means 12 heats the collection means 11 to a high temperature state in which the sample gas collected by the collection means 11 is desorbed according to the control of the first control means 16a and the like.

中空状部材１３は、熱伝導性部材等によって中空円柱状のバッファとして形成されており、ステンレス配管等が用いられる。中空状部材１３は、試料ガスの流れ方向Ｆの配管１０ａにおける捕集手段１１の下流側に、配管１０ａの一部として組み込まれている。   The hollow member 13 is formed as a hollow cylindrical buffer by a thermally conductive member or the like, and a stainless steel pipe or the like is used. The hollow member 13 is incorporated as a part of the pipe 10a on the downstream side of the collecting means 11 in the pipe 10a in the flow direction F of the sample gas.

切り替え手段１４は、第２制御手段１６ｂと電気的に接続されており、その第２制御手段１６ｂ等の制御に応じて、中空状部材１３を捕集手段１１からの気体の流通が不可能な閉塞状態とその流通が可能な開放状態に切り替える。切り替え手段１４は、捕集手段１１の上流側の配管１０ａに設けられた上流側弁１４ａと、中空状部材１３の下流側の配管１０ａに設けられた下流側弁１４ｂと、を有している。   The switching means 14 is electrically connected to the second control means 16b, and the flow of gas from the collecting means 11 through the hollow member 13 is impossible in accordance with the control of the second control means 16b and the like. Switch between the closed state and the open state where the flow is possible. The switching means 14 has an upstream valve 14 a provided in the pipe 10 a upstream of the collecting means 11 and a downstream valve 14 b provided in the pipe 10 a downstream of the hollow member 13. .

上流側弁１４ａと下流側弁１４ｂとの双方によって配管１０ａを遮断することで、捕集手段１１及び中空状部材１３は試料ガス等の気体の流通が不可能な閉塞状態となり、また、上流側弁１４ａと下流側弁１４ｂとの双方によって配管１０ａを開放することで、捕集手段１１及び中空状部材１３は試料ガス等の気体の流通が可能な開放状態となる。   By shutting off the pipe 10a by both the upstream valve 14a and the downstream valve 14b, the collecting means 11 and the hollow member 13 are in a closed state in which gas such as sample gas cannot flow, and the upstream side By opening the pipe 10a by both the valve 14a and the downstream valve 14b, the collecting means 11 and the hollow member 13 are in an open state in which a gas such as a sample gas can flow.

このように切り替え手段１４を構成することで、本実施形態では捕集手段１１及び中空状部材１３の双方を閉塞状態とする場合について説明するが、本発明はこれに限定するものではなく、例えば、上流側弁１４ａを捕集手段１１と中空状部材１３との間の配管１０ａに設けて、中空状部材１３のみを閉塞状態とするなど種々異なる実施形態とすることができる。   By configuring the switching means 14 in this way, in this embodiment, the case where both the collecting means 11 and the hollow member 13 are closed will be described, but the present invention is not limited to this, for example, The upstream valve 14a may be provided in the pipe 10a between the collecting means 11 and the hollow member 13 so that only the hollow member 13 is closed.

冷却手段１５は、第１制御手段１６ａと電気的に接続されており、公知であるクーラー、ペルチェ素子、等の冷却装置が用いられる。冷却手段１５は、第１制御手段１６ａ等の制御により、閉塞状態の中空状部材１３を冷却する。   The cooling means 15 is electrically connected to the first control means 16a, and a known cooling device such as a cooler or a Peltier element is used. The cooling means 15 cools the closed hollow member 13 under the control of the first control means 16a and the like.

第１制御手段１６ａ及び第２制御手段１６ｂは、マイクロ・コンピュータ等がプログラムの実行によって各種手段として機能する。第１制御手段１６ａは、試料ガスを捕集した捕集手段１１を加熱手段１２に加熱させ且つ中空状部材１３を冷却手段１５に冷却させる制御を行う手段である。第２制御手段１６ｂは、第１制御手段１６ａが捕集手段１１を加熱させ、中空状部材１３を冷却させた後に、中空状部材１３を開放状態へ切り替え手段１４に切り替えさせる制御を行う手段である。   The first control unit 16a and the second control unit 16b function as various units when a microcomputer or the like executes a program. The first control unit 16 a is a unit that performs control to cause the heating unit 12 to heat the collection unit 11 that has collected the sample gas and to cool the hollow member 13 to the cooling unit 15. The second control means 16b is a means for controlling the switching of the hollow member 13 to the open state after the first control means 16a heats the collecting means 11 and cools the hollow member 13. is there.

排出手段１７は、公知であるポンプ等が用いられ、第２制御手段１６ｂの制御に応じて捕集手段１１から脱離した濃縮ガスを中空状部材１３の下流側に排出するための手段である。本実施形態では、図１に示すように、排出手段１７を中空状部材１３の下流側に設ける場合について説明するが、本発明はこれに限定するものではなく、ポンプ等を捕集手段１１の上流側に設けるなど種々異なる実施形態とすることができる。また、中空状部材１３に捕集した試料ガスの脱離を促すために、冷却手段１５にヒーター等の加熱装置を追加することもできる。   The discharge means 17 is a means for discharging a concentrated gas desorbed from the collection means 11 to the downstream side of the hollow member 13 using a known pump or the like under the control of the second control means 16b. . In the present embodiment, as shown in FIG. 1, the case where the discharge means 17 is provided on the downstream side of the hollow member 13 will be described. However, the present invention is not limited to this, and a pump or the like is provided for the collection means 11. It can be set as various different embodiments, such as providing in an upstream. In addition, a heating device such as a heater can be added to the cooling means 15 in order to promote the detachment of the sample gas collected in the hollow member 13.

ここで、このような構成の試料ガス捕集装置１０における、脱離時の減圧作用について説明する。   Here, the decompression action at the time of desorption in the sample gas collecting apparatus 10 having such a configuration will be described.

捕集手段１１の捕集剤表面への気体分子の吸着量Ｍは、温度Ｔ、気体の圧力ｐ及び固体と気体間の吸着（捕集）相互作用ポテンシャルＥに依存するため、温度一定の場合、Ｍ＝ｆ（ｐ）T,Eで示す圧力の関数になり、また、圧力一定の場合、Ｍ＝ｆ（Ｔ）p,Eとなり、温度に依存する。このことから、低温で試料ガスを捕集し、高温低圧で脱離する方法を実現することができる。 The adsorption amount M of gas molecules on the surface of the collection agent 11 of the collection means 11 depends on the temperature T, the pressure p of the gas, and the adsorption (collection) interaction potential E between the solid and the gas. , M = f (p) T, E , and when the pressure is constant, M = f (T) p, E , which depends on the temperature. From this, it is possible to realize a method of collecting the sample gas at a low temperature and desorbing it at a high temperature and a low pressure.

まず、冷却時の中空状部材１３の温度を４０℃とし、加熱時を３５３℃とした場合、中空状部材１３の容量は５ｃｃで捕集手段１１と配管容量は十分に小さく無視できるものとする。そして、シャルルの法則より、ｔ℃のときの体積Ｖは式１で示される。なお、式１において、Ｖ０は０℃のときの体積、ｔは温度をそれぞれ示している、そして、この式１に基づいた、温度と体積の関係を表１に示している。
Ｖ＝Ｖ０＊（ｔ／２７３．１５＋１） ・・・ 式１ First, when the temperature of the hollow member 13 at the time of cooling is 40 ° C. and the temperature at the time of heating is 353 ° C., the capacity of the hollow member 13 is 5 cc and the collection means 11 and the pipe capacity are sufficiently small and can be ignored. . Then, according to Charles' law, the volume V at t ° C. is expressed by Equation 1. In Equation 1, V0 represents the volume at 0 ° C., t represents the temperature, and Table 1 shows the relationship between temperature and volume based on Equation 1.
V = V0 * (t / 273.15 + 1) Formula 1

Figure 2010096665
Figure 2010096665

表１に示すように、０℃で２．１８ｃｃの気体は、４０℃で２．５ｃｃ、３５３℃で５ｃｃであることから、５ｃｃの中空状部材１３は、３５３℃に加熱され、その状態で切り替え手段１４によって閉塞状態にされた後、４０℃に冷却されると、中空状部材１３の内部の気体は１／２に収縮されることになる。しかし、中空状部材１３は閉塞状態であるため、収縮できずにその内部が１／２に減圧されることになる。このような中空状部材１３の減圧作用を本発明では利用している。   As shown in Table 1, the 2.18 cc gas at 0 ° C. is 2.5 cc at 40 ° C. and 5 cc at 353 ° C. Therefore, the 5 cc hollow member 13 is heated to 353 ° C. After being closed by the switching means 14, when cooled to 40 ° C., the gas inside the hollow member 13 is shrunk by half. However, since the hollow member 13 is in a closed state, the hollow member 13 cannot be shrunk and its inside is decompressed to ½. Such a decompression action of the hollow member 13 is utilized in the present invention.

このような試料ガス捕集装置１０は、捕集手段１１に試料ガスが流れ込むと、捕集手段１１がその試料ガスを捕集する。試料ガス捕集装置１０は、上流側弁１４ａを遮断して捕集手段１１を加熱手段１２によって加熱し、下流側弁１４ｂを遮断して中空状部材１３を冷却手段１５によって冷却する。試料ガス捕集装置１０は、上流側弁１４ａを開放することで、捕集手段１１に捕集した試料ガスを中空状部材１３内に瞬間的に脱離させる。そして、試料ガス捕集装置１０は、下流側弁１４ｂを開放し、中空状部材１３内に脱離させた濃縮ガスを排出手段１７によって中空状部材１３の下流側に排出させる。   In such a sample gas collection device 10, when the sample gas flows into the collection means 11, the collection means 11 collects the sample gas. The sample gas collecting apparatus 10 shuts off the upstream valve 14 a and heats the collecting means 11 with the heating means 12, shuts off the downstream valve 14 b and cools the hollow member 13 with the cooling means 15. The sample gas collection device 10 opens the upstream side valve 14 a to instantaneously desorb the sample gas collected by the collection means 11 into the hollow member 13. Then, the sample gas collection device 10 opens the downstream side valve 14 b and discharges the concentrated gas desorbed into the hollow member 13 to the downstream side of the hollow member 13 by the discharge means 17.

以上説明した本発明の試料ガス捕集装置１０によれば、捕集手段１１の下流に中空状部材１３を設け、試料ガスを捕集した捕集手段１１を加熱し、中空状部材１３を冷却した後に、捕集手段１１と中空状部材１３を流通させるように切り替えることから、高温状態の捕集手段１１内は一気に低圧力に変化するため、捕集手段１１に有効な負圧効果を得ることが可能となり、捕集手段から試料ガスを極短時間で脱離させることができる。従って、その脱離した濃縮ガスを排出するのに必要なキャリアガス（パージガス）が少量で良いため、試料ガスの分離性を低下させることなく、十分な脱離効果を得ることができる。   According to the sample gas collecting apparatus 10 of the present invention described above, the hollow member 13 is provided downstream of the collecting means 11, the collecting means 11 collecting the sample gas is heated, and the hollow member 13 is cooled. After that, since the collecting means 11 and the hollow member 13 are switched to flow, the inside of the collecting means 11 in a high temperature state is changed to a low pressure at a stretch, so that an effective negative pressure effect is obtained for the collecting means 11. Thus, the sample gas can be desorbed from the collecting means in a very short time. Accordingly, since a small amount of carrier gas (purge gas) is required for discharging the desorbed concentrated gas, a sufficient desorption effect can be obtained without degrading the separation of the sample gas.

また、試料ガス捕集装置１０によれば、捕集手段１１の上流側に上流側弁１４ａを設けるようにしたことから、捕集手段１１を中空状部材１３と共に減圧させることができるため、捕集手段１１から試料ガスをより一層短時間で脱離させることができる。   In addition, according to the sample gas collecting device 10, since the upstream valve 14a is provided on the upstream side of the collecting means 11, the collecting means 11 can be decompressed together with the hollow member 13; The sample gas can be desorbed from the collecting means 11 in a shorter time.

次に、上述した試料ガス捕集装置１０をガスクロマトグラフ装置に適用する場合の一実施例を、以下に説明する。なお、上述した試料ガス捕集装置１０と共通する部分には同一の符号を付し、重複する説明は省略する。   Next, an example in which the above-described sample gas collecting apparatus 10 is applied to a gas chromatograph apparatus will be described below. In addition, the same code | symbol is attached | subjected to the part which is common in the sample gas collection apparatus 10 mentioned above, and the overlapping description is abbreviate | omitted.

図２において、ガスクロマトグラフ装置（以下、ＧＣ装置）１は、捕集手段１１と、第１加熱冷却手段１２と、中空状部材１３と、切り替え手段１４と、第２加熱冷却手段１５と、制御手段１６と、排出手段１７と、分離手段１８と、検出手段１９と、活性炭フィルタ２０と、を有して構成している。   In FIG. 2, a gas chromatograph apparatus (hereinafter referred to as GC apparatus) 1 includes a collection means 11, a first heating / cooling means 12, a hollow member 13, a switching means 14, a second heating / cooling means 15, and a control. Means 16, discharge means 17, separation means 18, detection means 19, and activated carbon filter 20 are included.

ＧＣ装置１はさらに、上述した配管１０ａと、試料ガスを吸気する第１配管１０ｂと、キャリアガス（パージガス）等を吸気する第２配管１０ｃと、配管１０ａに第１配管１０ｂと第２配管１０ｃとを選択的に流通させるための三方弁Ｖと、を有している。   The GC apparatus 1 further includes the above-described pipe 10a, the first pipe 10b for sucking the sample gas, the second pipe 10c for sucking the carrier gas (purge gas), and the like, and the pipe 10a with the first pipe 10b and the second pipe 10c. And a three-way valve V for selectively circulating.

三方弁Ｖは、３つのポートａ、ｂ、ｃを備え、ポートａには第１配管１０ｂ、ポートｂには第２配管１０ｃ、ポートｃには配管１０ａがそれぞれ接続されている。三方弁Ｖは、制御手段１６の制御によって切り替えられ、試料ガスの導入に応じて、第１配管１０ｂと配管１０ａとを接続し（ａ−ｃ接続）、キャリアガスの導入に応じて、第２配管１０ｃと配管１０ａとを接続する（ｂ−ｃ接続）。   The three-way valve V includes three ports a, b, and c. A first pipe 10b is connected to the port a, a second pipe 10c is connected to the port b, and a pipe 10a is connected to the port c. The three-way valve V is switched by the control of the control means 16, and connects the first pipe 10b and the pipe 10a (acc connection) in accordance with the introduction of the sample gas (second connection), and the second in accordance with the introduction of the carrier gas. The pipe 10c and the pipe 10a are connected (bc connection).

第１加熱冷却手段１２は、図示しないが、上述した加熱手段１２に相当する加熱装置と、冷却装置と、を有している。加熱装置は、制御手段１６の制御によって、捕集手段１１に捕集された試料ガスの脱離を促すように捕集手段１１を加熱する。冷却装置は、制御手段１６の制御によって、捕集手段１１に導入された試料ガスの捕集を促すように捕集手段１１を冷却する。   Although not shown, the first heating / cooling unit 12 includes a heating device corresponding to the heating unit 12 described above and a cooling device. The heating device heats the collection means 11 under the control of the control means 16 so as to promote the desorption of the sample gas collected by the collection means 11. The cooling device cools the collection unit 11 under the control of the control unit 16 so as to encourage collection of the sample gas introduced into the collection unit 11.

切り替え手段１４は、上述した上流側弁１４ａと、三方弁である下流側弁１４ｂと、を有している。この下流側弁１４ｂは、３つのポートａ、ｂ、ｃを備え、ポートａ、ｃには配管１０ａ、ポートｂには第２配管１０ｃがそれぞれ接続されている。下流側弁１４ｂは、制御手段１６の制御によって切り替えられ、試料ガスの流通時等は、配管１０ａ同士を接続し（ａ−ｃ接続）、キャリアガスの流通時等は、第２配管１０ｃと配管１０ａとを接続する（ｂ−ｃ接続）。   The switching means 14 has the upstream valve 14a described above and a downstream valve 14b that is a three-way valve. The downstream valve 14b includes three ports a, b, and c. A pipe 10a is connected to the ports a and c, and a second pipe 10c is connected to the port b. The downstream side valve 14b is switched under the control of the control means 16, and the pipes 10a are connected to each other when the sample gas flows (ac connection), and the second pipe 10c and the pipe are connected when the carrier gas flows. 10a is connected (bc connection).

第２加熱冷却手段１５は、第１加熱冷却手段１２と同一構成であり、加熱装置と、上述した冷却手段１２に相当する冷却装置と、を有している。加熱装置は、制御手段１６の制御によって、中空状部材１３に捕集された試料ガスの脱離を促すように中空状部材１３を加熱する。この中空状部材１３の加熱は、内部の空気を膨張させ、予め下流側弁１４ｂから上記の膨張分の空気を排気させることで、後の減圧作用をより効果的にすることができる。また、冷却装置は、制御手段１６の制御によって、中空状部材１３の減圧作用を促すように中空状部材１３を冷却する。   The second heating / cooling means 15 has the same configuration as the first heating / cooling means 12, and includes a heating device and a cooling device corresponding to the cooling means 12 described above. The heating device heats the hollow member 13 under the control of the control means 16 so as to promote the detachment of the sample gas collected in the hollow member 13. The heating of the hollow member 13 can expand the internal air and exhaust the air corresponding to the expansion from the downstream valve 14b in advance, thereby making the subsequent decompression effect more effective. In addition, the cooling device cools the hollow member 13 so as to promote the pressure reducing action of the hollow member 13 under the control of the control means 16.

制御手段１６は、ＣＰＵ（中央処理装置）、ＲＯＭ（読み出し専用メモリ）、及びＲＡＭ（随時書き込み読み出しメモリ）を有するマイクロプロセッサユニット等で構成されている。そして、制御手段１６は、試料ガス捕集装置１０、分離手段１８、検出手段１９、三方弁Ｖ等に電気的に接続され、各々の制御を行う。   The control means 16 includes a microprocessor unit having a CPU (Central Processing Unit), a ROM (Read Only Memory), and a RAM (A Write / Read Memory as needed). And the control means 16 is electrically connected to the sample gas collection apparatus 10, the separation means 18, the detection means 19, the three-way valve V, etc., and performs each control.

制御手段１６は、ＲＯＭ等に上述した第１制御手段１６ａ及び第２制御手段１６ｂとしてＣＰＵ（コンピュータ）を機能させるためのプログラムを記憶している。制御手段１６は、検出手段１９からのセンサ出力を所定のサンプリング間隔で取得し、それらのセンサ出力に基づいて、分離手段１８で分離した試料ガスの各分離ガスの濃度を算出して、試料ガスを分析する。即ち、制御手段１６は、特許請求の範囲に記載の分析手段として機能しているが、本発明はこれに限定するものではなく、検出手段１９に分析機能として組み込まれるるなど種々異なる実施例とすることができる。   The control means 16 stores a program for causing a CPU (computer) to function as the first control means 16a and the second control means 16b described above in a ROM or the like. The control means 16 acquires the sensor output from the detection means 19 at a predetermined sampling interval, calculates the concentration of each separation gas of the sample gas separated by the separation means 18 based on these sensor outputs, and the sample gas Analyze. That is, the control means 16 functions as the analysis means described in the claims. However, the present invention is not limited to this, and various embodiments such as being incorporated in the detection means 19 as an analysis function. can do.

分離手段１８は、公知であるガスクロマトグラフの分離カラム等が用いられる。分離手段１８は、ヒータによって加熱されることで、導入された濃縮ガス（試料ガス）をその種類（測定対象成分）により時間軸上（所定の測定期間）で分離して送出する。   The separation means 18 is a known gas chromatograph separation column or the like. The separating means 18 is heated by a heater, and the introduced concentrated gas (sample gas) is separated on the time axis (predetermined measurement period) according to the type (component to be measured) and sent out.

検出手段１９は、例えば、接触燃焼式ガスセンサ、吸着燃焼式ガスセンサ等が任意に用いられる。検出手段１９は、例えば感応素子部と感応素子部の抵抗差に基づいて、ガス濃度を示すセンサ信号を制御手段１６に出力する。   As the detection means 19, for example, a contact combustion type gas sensor, an adsorption combustion type gas sensor or the like is arbitrarily used. The detection unit 19 outputs a sensor signal indicating the gas concentration to the control unit 16 based on, for example, a resistance difference between the sensitive element unit and the sensitive element unit.

活性炭フィルタ２０は、大気口から大気を吸入して、フィルタ内の活性炭により大気に含まれる不純物を取り除いてキャリアガスを生成するものである。   The activated carbon filter 20 sucks the atmosphere from the atmosphere port, removes impurities contained in the atmosphere with activated carbon in the filter, and generates a carrier gas.

次に、ＧＣ装置１の本発明に係る処理概要の一例を、図３乃至図１０の図面を参照して以下に説明する。   Next, an example of a processing outline of the GC apparatus 1 according to the present invention will be described below with reference to the drawings of FIGS.

ガスクロマトグラフ装置１は、電源投入により起動されると、クリーニング工程Ｓ１において（図５参照）、三方弁Ｖをｂ−ｃに接続に切り替え、上流側弁１４ａを導通させ、下流側弁１４ｂをａ−ｃ接続に切り替え、そして、排出手段１７を作動させることで、測定誤差をなくすために、吸気口から吸気した外気又は清浄空気を活性炭フィルタ２０を通してガス成分や湿度を除去したキャリアガス（パージガス）として、第２流路１０ｃから流路１０ａを流通させて排出手段１７から排出させる。   When the gas chromatograph apparatus 1 is activated by turning on the power, in the cleaning step S1 (see FIG. 5), the three-way valve V is switched to connection b-c, the upstream valve 14a is turned on, and the downstream valve 14b is switched to a. In order to eliminate measurement errors by switching to the -c connection and operating the discharge means 17, the carrier gas (purge gas) from which the outside air or clean air taken in from the intake port is removed from the gas component and humidity through the activated carbon filter 20 As a result, the flow path 10 a is circulated from the second flow path 10 c and discharged from the discharge means 17.

サンプリング工程Ｓ２において（図６参照）、三方弁Ｖをａ−ｃに接続に切り替え、上流側弁１４ａを導通させ、下流側弁１４ｂをａ−ｃ接続に切り替え、第１加熱冷却手段１２によって捕集手段１１を冷却する。なお、第２加熱冷却手段１５によって中空状部材１３を加熱する。そして、捕集手段１１の冷却が完了したら、所定の期間（容量）分だけ排出手段１７を作動させることで、第１流路１０ｂから導入した試料ガスを捕集手段１１に流し込む。これにより、捕集手段１１に試料ガスを捕集することができる。   In the sampling step S2 (see FIG. 6), the three-way valve V is switched to ac connection, the upstream valve 14a is conducted, the downstream valve 14b is switched to ac connection, and captured by the first heating / cooling means 12. The collecting means 11 is cooled. The hollow member 13 is heated by the second heating / cooling means 15. Then, when the cooling of the collection means 11 is completed, the sample gas introduced from the first flow path 10b is poured into the collection means 11 by operating the discharge means 17 for a predetermined period (capacity). Thereby, the sample gas can be collected in the collecting means 11.

脱離１工程Ｓ３において（図７参照）、下流側弁１４ｂをａ−ｃ接続状態のまま、上流側弁１４ａを遮断することで、捕集手段１１及び中空状部材１３を導通させ、第１加熱冷却手段１２によって捕集手段１１を加熱する。これにより、捕集手段１１は、試料ガスの捕集を促す高温状態となる。なお、上流側弁１４ａから排出手段１７前の流路１０ａを減圧させて捕集手段１１からの脱離を促進するように排出手段１７を作動させてもよい。   In the detachment 1 step S3 (see FIG. 7), the upstream valve 14a is shut off while the downstream valve 14b remains in the ac connection state, whereby the collecting means 11 and the hollow member 13 are made conductive. The collecting means 11 is heated by the heating / cooling means 12. Thereby, the collection means 11 will be in the high temperature state which encourages collection of sample gas. Note that the discharge means 17 may be operated so as to promote the detachment from the collection means 11 by reducing the pressure of the flow path 10a before the discharge means 17 from the upstream valve 14a.

脱離２工程Ｓ４において（図８参照）、上流側弁１４ａを遮断させ、下流側弁１４ｂをｂ−ｃ接続に切り替え（遮断させ）、排出手段１７を停止する。そして、第２加熱冷却手段１５によって中空状部材１３を冷却する。これにより、中空状部材１３内は、冷却によって気体が収縮されて減圧されることになる。   In the desorption 2 step S4 (see FIG. 8), the upstream valve 14a is shut off, the downstream valve 14b is switched (blocked) to the bc connection, and the discharge means 17 is stopped. Then, the hollow member 13 is cooled by the second heating / cooling means 15. As a result, the inside of the hollow member 13 is depressurized by contraction of the gas by cooling.

脱離３工程Ｓ５において（図９参照）、上流側弁１４ａを導通させることで、捕集手段１１内に捕集した試料ガスは、上流側弁１４ａが開いた瞬間に、中空状部材１３内に向かって脱離される。これにより、脱離した試料ガスは、中空状部材１３内に濃縮ガスＧとして導入されて捕集される。   In the desorption 3 step S5 (see FIG. 9), the sample gas collected in the collecting means 11 by conducting the upstream side valve 14a is transferred into the hollow member 13 at the moment when the upstream side valve 14a is opened. It is desorbed toward. Thereby, the desorbed sample gas is introduced into the hollow member 13 as the concentrated gas G and collected.

打込み工程Ｓ６において（図１０参照）、第１加熱冷却手段１２によって捕集手段１１を冷却し、第２加熱冷却手段１５によって中空状部材１３を加熱する。そして、排出手段１７を作動させることで、中空状部材１３内に脱離した濃縮ガスＧを分離手段１８に排出する。これにより、濃縮ガスＧが分離手段１８に導入されることになる。なお、下流側弁１４ｂの導通状態への切り替えのタイミングについては、図４に示すように、中空状部材１３の冷却／加熱の前後の間に切り替える。   In the driving step S <b> 6 (see FIG. 10), the collecting means 11 is cooled by the first heating / cooling means 12, and the hollow member 13 is heated by the second heating / cooling means 15. Then, by operating the discharge means 17, the concentrated gas G desorbed in the hollow member 13 is discharged to the separation means 18. As a result, the concentrated gas G is introduced into the separation means 18. In addition, about the timing of the switching to the conduction | electrical_connection state of the downstream valve 14b, as shown in FIG. 4, it switches between before and after cooling / heating of the hollow member 13. As shown in FIG.

分析工程Ｓ７において、下流側弁１４ｂをｂ−ｃ接続に切り替え、排出手段１７を作動させることで、上記キャリアガスを分離手段１８へ流通させて、濃縮ガスＧを分離手段１８で試料ガス成分に分離させる。そして、キャリアガスによって、それぞれの試料ガス成分が時間差をもって検出手段１９のガスセンサに搬送されて、各成分の検出が行われる。そして、検出手段１９がセンサ信号を制御手段１６に出力すると、制御手段１６によって分離手段１８で分離した各分離ガスの濃度を算出して試料ガスを分析する。そして、全ての検出対象成分の分析が終了すると、上述した一連の工程を繰り返す。   In the analysis step S7, the downstream valve 14b is switched to the bc connection and the discharge means 17 is operated, whereby the carrier gas is circulated to the separation means 18, and the concentrated gas G is converted into the sample gas component by the separation means 18. Separate. Then, each sample gas component is conveyed to the gas sensor of the detection means 19 with a time difference by the carrier gas, and each component is detected. When the detection means 19 outputs a sensor signal to the control means 16, the control means 16 calculates the concentration of each separation gas separated by the separation means 18 and analyzes the sample gas. When the analysis of all the detection target components is completed, the series of steps described above is repeated.

以上説明した本発明のガスクロマトグラフ装置１によれば、捕集した試料ガスの分離性を向上させ且つ短時間で高濃度の試料ガスを送出する試料ガス捕集装置１０の構成を有していることから、中空状部材１３から検出手段１９（分析手段）に短時間で高濃度の試料ガスを送出することができ、分析手段は急激な検出ピークを得ることができるため、ガスの成分を効率的に分析することができる。従って、高精度で再現性の良い測定が可能となり、試料ガスの分析に要するランニングコストを削減することができる。   According to the gas chromatograph apparatus 1 of the present invention described above, the configuration of the sample gas collecting apparatus 10 that improves the separability of the collected sample gas and delivers a high concentration sample gas in a short time is provided. Therefore, a high concentration of sample gas can be sent from the hollow member 13 to the detection means 19 (analysis means) in a short time, and the analysis means can obtain a sudden detection peak, so that the gas components can be efficiently used. Analysis. Therefore, measurement with high accuracy and good reproducibility is possible, and the running cost required for analyzing the sample gas can be reduced.

なお、上述した各実施形態は本発明の代表的な形態を示したに過ぎず、本発明は、実施形態に限定されるものではない。即ち、本発明の骨子を逸脱しない範囲で種々変形して実施することができる。   The above-described embodiments are merely representative examples of the present invention, and the present invention is not limited to the embodiments. That is, various modifications can be made without departing from the scope of the present invention.

本発明の試料ガス捕集装置の基本構成を示す構成図である。It is a block diagram which shows the basic composition of the sample gas collection apparatus of this invention. 本発明のガスクロマトグラフ装置の概略構成の一例を示す構成図である。It is a block diagram which shows an example of schematic structure of the gas chromatograph apparatus of this invention. ガスクロマトグラフ装置の本発明に係る処理工程の一例を示すフローチャートである。It is a flowchart which shows an example of the process process which concerns on this invention of a gas chromatograph apparatus. 図３の処理工程に対応したタイミングチャートである。4 is a timing chart corresponding to the processing step of FIG. 3. 図３中のクリーニング工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the cleaning process in FIG. 図３中のサンプリング工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the sampling process in FIG. 図３中の脱離１工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the detachment | desorption 1 process in FIG. 図３中の脱離２工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the detachment | desorption 2 process in FIG. 図３中の脱離３工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the detachment | desorption 3 process in FIG. 図３中の打込み工程における動作状態を説明するための図である。It is a figure for demonstrating the operation state in the implantation process in FIG. 従来のガスクロマトグラフ装置の構成図である。It is a block diagram of the conventional gas chromatograph apparatus.

符号の説明Explanation of symbols

１ ガスクロマトグラフ装置
１０ 試料ガス捕集装置
１０ａ 配管
１１ 捕集手段
１２ 加熱手段（第１加熱冷却手段）
１３ 中空状部材
１４ 切り替え手段
１５ 冷却手段（第２加熱冷却手段）
１６ａ 第１制御手段
１６ｂ 第２制御手段
１７ 排出手段
１９ 検出手段（分析手段） DESCRIPTION OF SYMBOLS 1 Gas chromatograph apparatus 10 Sample gas collection apparatus 10a Piping 11 Collection means 12 Heating means (1st heating-cooling means)
13 Hollow member 14 Switching means 15 Cooling means (second heating and cooling means)
16a First control means 16b Second control means 17 Discharge means 19 Detection means (analysis means)

Claims (3)

配管に設けられて前記配管内を流れる試料ガスを捕集する捕集手段と、前記捕集手段に捕集した試料ガスが脱離する高温状態に前記捕集手段を加熱する加熱手段と、を有する試料ガス捕集装置において、
前記試料ガスの流れ方向の前記配管における前記捕集手段の下流側に設けられた中空状部材と、
前記中空状部材を前記捕集手段からの気体の流通が不可能な閉塞状態とその流通が可能な開放状態に切り替える切り替え手段と、
前記中空状部材が閉塞状態のときに前記中空状部材を冷却する冷却手段と、
前記試料ガスを捕集した捕集手段を前記加熱手段に加熱させ且つ前記中空状部材を前記冷却手段に冷却させる第１制御手段と、
前記第１制御手段が前記捕集手段を加熱させ且つ前記中空状部材を冷却させた後に、前記中空状部材を開放状態へ前記切り替え手段に切り替えさせる第２制御手段と、
前記第２制御手段による制御に応じて前記捕集手段から脱離した濃縮ガスを排出させる排出手段と、
を有することを特徴とする試料ガス捕集装置。 A collecting means for collecting a sample gas provided in a pipe and flowing in the pipe; and a heating means for heating the collecting means to a high temperature state where the sample gas collected in the collecting means is desorbed. In a sample gas collector having
A hollow member provided on the downstream side of the collecting means in the pipe in the flow direction of the sample gas;
Switching means for switching the hollow member between a closed state in which gas cannot be circulated from the collecting means and an open state in which the circulation is possible;
Cooling means for cooling the hollow member when the hollow member is closed;
First control means for causing the heating means to heat the collecting means for collecting the sample gas and cooling the hollow member to the cooling means;
After the first control means heats the collecting means and cools the hollow member, the second control means to switch the hollow member to the switching means to an open state;
A discharge means for discharging the concentrated gas desorbed from the collection means according to the control by the second control means;
A sample gas collecting device comprising: 前記切り替え手段が、前記捕集手段の上流側の前記配管に設けられた上流側弁と、前記中空状部材の下流側の前記配管に設けられた下流側弁と、を有することを特徴とする請求項１に記載の試料ガス捕集装置。   The switching means includes an upstream valve provided in the pipe upstream of the collecting means, and a downstream valve provided in the pipe downstream of the hollow member. The sample gas collection device according to claim 1. 請求項１又は２に記載の試料ガス捕集装置と、前記試料ガス捕集装置で脱離した試料ガスの成分を分析する分析手段と、を有することを特徴とするガスクロマトグラフ装置。   A gas chromatograph device comprising: the sample gas collection device according to claim 1; and an analysis unit that analyzes a component of the sample gas desorbed by the sample gas collection device.
JP2008268715A 2008-10-17 2008-10-17 Sample gas collector and gas chromatograph device Withdrawn JP2010096665A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108593816A (en) * 2018-04-28 2018-09-28 江苏中烟工业有限责任公司 A kind of method and device improving volatile ingredient purging efficiency in tobacco
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

Cited By (4)

* Cited by examiner, † Cited by third party
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
JP7214687B2 (en) 2016-03-08 2023-01-30 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 sampling device and method
US11896366B2 (en) 2018-03-06 2024-02-13 Entech Instruments Inc. Ventilator-coupled sampling device and method
CN108593816A (en) * 2018-04-28 2018-09-28 江苏中烟工业有限责任公司 A kind of method and device improving volatile ingredient purging efficiency in tobacco

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