JP4089646B2 - Organic volatile matter collection tube and organic volatile matter measurement method - Google Patents

Organic volatile matter collection tube and organic volatile matter measurement method Download PDF

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JP4089646B2
JP4089646B2 JP2004099846A JP2004099846A JP4089646B2 JP 4089646 B2 JP4089646 B2 JP 4089646B2 JP 2004099846 A JP2004099846 A JP 2004099846A JP 2004099846 A JP2004099846 A JP 2004099846A JP 4089646 B2 JP4089646 B2 JP 4089646B2
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collection tube
test piece
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thermal desorption
volatile matter
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JP2005283429A (en
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修一 石割
得男 久▲禮▼
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Hitachi Plant Technologies Ltd
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本発明は有機揮発物測定用捕集管及び有機揮発物測定方法に係り、特に有機材料などの試験片から微量に揮発する吸着性の強い有機揮発物を測定する場合に好適な有機揮発物測定用捕集管及び有機揮発物測定方法に関する。   The present invention relates to a collection tube for organic volatile matter measurement and an organic volatile matter measurement method, and particularly suitable for measuring highly adsorbable organic volatile matter that volatilizes in a trace amount from a test piece such as an organic material. The present invention relates to a collection tube for use and an organic volatile matter measuring method.

クリーンルームを構成する壁材や床材又はクリーンルーム内に設置される各種機器にはさまざまな有機材料が使用されている。これらの有機材料から有機揮発物が発生する。代表的なものとしてジオクチルフタル酸(DOP)がある。このジオクチルフタル酸はプラスチック材中の可塑性の添加剤として多く使用される。ジオクチルフタル酸の性質は沸点が360℃であり、常温ではわずかに揮発する。このためジオクチルフタル酸は通常クリーンルーム雰囲気中には0.1から1ng/Lの微量含まれている。ジブチルフタル酸(DBP)やジオクチルアジピン酸(DOA)なども同様にクリーンルーム雰囲気中に微量含まれている。クリーンルーム雰囲気中に存在するこれらの有機揮発物が半導体ウェハ表面に吸着し、その電気特性に影響を与える問題がある。そこで、このような有機揮発物のうちウェハ表面に吸着するものを評価する必要がある。   Various organic materials are used for various materials installed in wall materials and floor materials constituting clean rooms or clean rooms. Organic volatiles are generated from these organic materials. A typical example is dioctyl phthalic acid (DOP). Dioctyl phthalic acid is often used as a plastic additive in plastic materials. Dioctyl phthalic acid has a boiling point of 360 ° C. and is slightly volatile at room temperature. For this reason, dioctylphthalic acid is usually contained in a trace amount of 0.1 to 1 ng / L in a clean room atmosphere. Dibutyl phthalic acid (DBP), dioctyl adipic acid (DOA), and the like are similarly contained in a clean room atmosphere. There is a problem that these organic volatiles present in the clean room atmosphere are adsorbed on the surface of the semiconductor wafer and affect the electrical characteristics thereof. Therefore, it is necessary to evaluate those organic volatiles that adsorb on the wafer surface.

現在、有機材料などの試験片から揮発する有機揮発物の測定は日本空気清浄協会の「クリーンルーム構成材料から発生する分子状汚染物質の測定方法指針(案)」で記述されている方法が使用されている。その概要図を図10に示した。この測定方法は、試験片1から揮発する有機揮発物を吸引ポンプ5により吸引し、積算流量計6で測定時間を調整しながら、気流にのせて吸引ポンプ手前の捕集部で捕集する方法である。まず、測定対象となる有機材料などの試験片1をチャンバー2に入れる。このチャンバー2の材質はステンレス製又はガラス製容器を使用している。チャンバー2内上部の注入口から清浄空気又は窒素ガスなどを注入し、試験片1から揮発する有機揮発物を気流に同伴させ、チャンバー2上部の排出口に接続された配管7を通じてインビンジャー3又は捕集剤4などの捕集部で捕集する。その後、捕集部に捕集された有機揮発物を熱脱着式ガスクロマトグラフなどによって分析し、有機揮発物の種類及び量を測定している。   Currently, the method described in “Measurement Guidelines for Molecular Pollutants Generated from Cleanroom Constituent Materials (Draft)” of the Japan Air Cleaning Association is used to measure organic volatiles volatilized from specimens such as organic materials. ing. A schematic diagram thereof is shown in FIG. In this measurement method, organic volatiles that are volatilized from the test piece 1 are sucked by the suction pump 5 and are collected by the collecting part in front of the suction pump on the air flow while adjusting the measurement time with the integrating flow meter 6. It is. First, a test piece 1 such as an organic material to be measured is placed in the chamber 2. The chamber 2 is made of a stainless steel or glass container. Purified air or nitrogen gas is injected from the upper inlet in the chamber 2, organic volatiles volatilized from the test piece 1 are entrained in the air flow, and the invinger 3 or the through the pipe 7 connected to the upper outlet of the chamber 2. Collected by a collection unit such as a collection agent 4. Thereafter, the organic volatiles collected in the collection part are analyzed by a thermal desorption gas chromatograph or the like, and the type and amount of the organic volatiles are measured.

また、特許文献1には汚染物質が吸着した試験片を吸着管容器に収容し、この吸着管容器ごと質量分析装置に装着することによって試験片に吸着された汚染物質の熱脱着を行い、汚染物質の種類及び質量を測定して被測定個所の汚染度を評価する方法が記載されている。
特開2001−264295号公報
Further, in Patent Document 1, a test piece on which contaminants are adsorbed is accommodated in an adsorption tube container, and by attaching the adsorption tube container to the mass spectrometer, the contaminants adsorbed on the test piece are thermally desorbed and contaminated. A method is described in which the type and mass of a substance are measured to evaluate the degree of contamination at the location to be measured.
JP 2001-264295 A

しかしながら前記指針による測定方法では、試験片から発生した有機揮発物のうち前記したジオクチルフタル酸(DOP)などの吸着性の強いものは、チャンバー2内部、又は配管7の内壁に吸着されてしまい、捕集部に到達できない。このため発生した有機揮発物の種類・量を精度良く測定することは困難である。また、特許文献1に記載された方法は試験片に吸着された汚染物質を測定し評価する方法であって、プラスチック構成材などの試験片から揮発する有機揮発物を測定するための方法ではない。   However, in the measurement method according to the guideline, organic volatiles generated from the test piece are strongly adsorbed such as dioctylphthalic acid (DOP), and are adsorbed on the inside of the chamber 2 or the inner wall of the pipe 7. Unable to reach the collecting part. For this reason, it is difficult to accurately measure the type and amount of generated organic volatiles. In addition, the method described in Patent Document 1 is a method for measuring and evaluating contaminants adsorbed on a test piece, and is not a method for measuring organic volatiles volatilized from a test piece such as a plastic component. .

本発明の目的は、試験片から揮発する吸着性の強い有機揮発物に対しても精度良く測定することが可能な有機揮発物測定用捕集管及び有機揮発物測定方法を提供することにある。   An object of the present invention is to provide a collection tube for measuring organic volatile matter and an organic volatile matter measuring method capable of accurately measuring even strongly adsorbing organic volatiles that volatilize from a test piece. .

上記目的を達成するために、本発明に係る有機揮発物測定用捕集管は、気流の流入口と流出口を備えた管状体と、この管状体の上流部に配置されて試験片を収容可能な試験片収容部と、前記管状体の下流部に配置された有機揮発物の捕集剤充填部と、前記試験片収容部と捕集剤充填部との中間に配置された有機揮発物の吸着部と、当該吸着部を通過する気流を管内壁に案内する気流案内部材とを具備し、熱脱着型ガスクロマトグラフ装置の熱脱着部に直接に装填可能とされたことを特徴とする。   In order to achieve the above object, an organic volatile matter measuring collection tube according to the present invention includes a tubular body provided with an airflow inlet and an outlet and an upstream portion of the tubular body for accommodating a test piece. A possible test piece container, an organic volatiles collector filling part disposed in the downstream part of the tubular body, and an organic volatile matter disposed between the test piece container and the collector filling part. And an airflow guide member for guiding the airflow passing through the adsorption portion to the inner wall of the pipe, and can be directly loaded into the thermal desorption portion of the thermal desorption type gas chromatograph apparatus.

また、本発明に係る有機揮発物測定用捕集管は、前記有機揮発物測定用捕集管が一次捕集管と二次捕集管に分割されており、一次捕集管には前記試験片収容部と前記吸着部と前記気流案内部材とが配置され、二次捕集管には前記捕集剤充填部が配置され、前記一次捕集管及び二次捕集管がそれぞれ単独で熱脱着型ガスクロマトグラフ装置の熱脱着部に装填可能とされたことを特徴とする。   In addition, the organic volatile matter measuring collection tube according to the present invention includes the organic volatile matter measuring collection tube divided into a primary collection tube and a secondary collection tube. A piece containing part, the adsorbing part, and the airflow guide member are arranged, the collecting agent filling part is arranged in a secondary collecting pipe, and the primary collecting pipe and the secondary collecting pipe are each heated independently. The desorption type gas chromatograph apparatus can be loaded into a thermal desorption section.

前記気流案内部材はフィルタ部材の中央部に気流遮断部材を配した構成とされ、管断面に対して前記気流を環状に案内するようにされた方が好ましい。
また、本発明に係る有機揮発物測定方法は、上記構成の捕集管を気流の流入口が上方に位置するように鉛直に配置し、前記試験片を前記流入口から吊り下げた状態で前記捕集管に収容し、当該捕集管内に空気を導入して前記試験片から揮発した有機揮発物を前記吸着部及び捕集剤充填部で吸着、捕集する第1工程と、第1工程後の捕集管から前記試験片を抜き出した後に、当該捕集管を熱脱着型ガスクロマトグラフ装置の熱脱着部に装填し、前記捕集管に吸着、捕集された有機揮発物を前記熱脱着型ガスクロマトグラフ装置によって分析する第2工程とを含むことを特徴とする。
It is preferable that the airflow guide member has a structure in which an airflow blocking member is disposed at a central portion of the filter member and guides the airflow in an annular shape with respect to a pipe cross section.
Further, in the organic volatile matter measuring method according to the present invention, the collection pipe having the above-described configuration is arranged vertically so that the airflow inlet is located above, and the test piece is suspended from the inlet. A first step in which the organic volatiles contained in the collection tube and introduced into the collection tube and volatilized from the test piece are adsorbed and collected by the adsorption unit and the collection agent filling unit; and a first step After extracting the test piece from the subsequent collection tube, the collection tube is loaded into a thermal desorption part of a thermal desorption type gas chromatograph device, and the organic volatiles adsorbed and collected in the collection tube are converted into the heat And a second step of analyzing by a desorption type gas chromatograph apparatus.

本発明によれば、試験片を捕集管に収容し、試験片から揮発した有機揮発物を即座に当該捕集管内で捕集し、この捕集管を熱脱着型ガスクロマトグラフ装置の熱脱着部に直接に装填可能にした。このため、試験片から揮発するジオクチルフタル酸(DOP)などの吸着性の強い有機揮発物に対しても精度良く測定することができる。特に吸着部を通過する気流を管内壁に案内する気流案内部材を配置することによって、捕集管を熱脱着型ガスクロマトグラフ装置の熱脱着部に装填し熱脱着を行う際には、キャリアガスが管内壁に吸着している有機揮発物と十分に接触し、有機揮発物を確実に脱着させる。このため、有機揮発物の脱着率を高くすることができ、熱脱着型ガスクロマトグラフ装置での測定精度を向上させることができる。   According to the present invention, the test piece is accommodated in the collection tube, and the organic volatiles volatilized from the test piece are immediately collected in the collection tube, and the collection tube is thermally desorbed in the thermal desorption type gas chromatograph apparatus. It was made possible to load directly in the part. For this reason, it can measure with high precision also to organic volatiles with strong adsorptivity, such as dioctyl phthalic acid (DOP) which volatilizes from a test piece. In particular, by arranging an airflow guide member that guides the airflow passing through the adsorption section to the inner wall of the pipe, when the collection pipe is loaded into the thermal desorption section of the thermal desorption type gas chromatograph apparatus, Fully contact with organic volatiles adsorbed on the inner wall of the tube to ensure desorption of organic volatiles. For this reason, the desorption rate of the organic volatile matter can be increased, and the measurement accuracy in the thermal desorption type gas chromatograph apparatus can be improved.

また、捕集管が一次捕集管と二次捕集管に分割されており、サンプリング時には両者を連結して使用し、測定・分析時には両者を切り離して一次捕集管及び二次捕集管をそれぞれ単独で熱脱着型ガスクロマトグラフ装置の熱脱着部に装填して測定・分析を行えるようにした。このため、試験片から揮発する有機揮発物の種類、量の測定のみならず、揮発した有機揮発物の吸着性に関する傾向を究明する場合に有効である。さらに、一次捕集管に試験片収容部と吸着部と気流案内部材を配置し、吸着部を通過する気流を管内壁に案内するようにした。このため、一次捕集管で捕集された吸着性の強い有機揮発物の熱脱着型ガスクロマトグラフ装置での測定精度を向上させることができる。   In addition, the collection tube is divided into a primary collection tube and a secondary collection tube. They are used by connecting both at the time of sampling, and separated between the primary collection tube and the secondary collection tube during measurement and analysis. Were individually loaded into the thermal desorption part of the thermal desorption type gas chromatograph so that measurement and analysis could be performed. For this reason, it is effective not only for measuring the type and amount of the organic volatiles that volatilize from the test piece, but also for determining the tendency of the adsorbability of the volatile organic volatiles. Furthermore, the test piece storage part, the adsorption part, and the airflow guide member are arranged in the primary collection tube, and the airflow passing through the adsorption part is guided to the inner wall of the pipe. For this reason, the measurement accuracy in the thermal desorption-type gas chromatograph apparatus of the highly adsorbable organic volatiles collected by the primary collection tube can be improved.

これによりクリーンルームを構成する有機材料などの選択と、クリーンルーム雰囲気で許容される有機揮発物量との関係を明確にすることができる。よってクリーンルーム構成材料の開発時に含有する有機揮発物の影響などへ指針を与えることが可能となる。   This makes it possible to clarify the relationship between the selection of organic materials and the like constituting the clean room and the amount of organic volatiles allowed in the clean room atmosphere. Therefore, it becomes possible to give a guide to the influence of organic volatiles contained in the development of clean room constituent materials.

本発明の実施形態を添付図面に従って説明する。図1は本発明に係る有機揮発物測定用捕集管の第1実施形態を示す断面図である。当該捕集管10は一次捕集管12と二次捕集管14とに分割されている。一次捕集管12は石英製の管状体で形成され、上端開口には気流の流入口であるガス供給栓16が取リ付けられ、上流部が試験片18を収容可能な試験片収容部20とされる。試験片収容部20の下方エリアは有機揮発物の吸着部22とされる。吸着部22には当該吸着部22を通過する気流を管内壁に案内する気流案内部材24が配置されている。気流案内部材24は管断面を塞ぐように配置した石英フィルタ24Aの中央部に気流遮断部材として石英板24Bを固定した構造であり、石英板24Bの側部と管内壁との間には環状の隙間Sが形成されている。吸着部を通過する気流は石英板24Bを避けて環状の隙間Sを通ることになり、その結果、気流は管内壁に案内される。気流案内部材24の下方は先細状のテーパ部26とされ、テーパ部26の下端に連結部28が形成されている。   Embodiments of the present invention will be described with reference to the accompanying drawings. FIG. 1 is a sectional view showing a first embodiment of a collection tube for measuring organic volatile matter according to the present invention. The collection tube 10 is divided into a primary collection tube 12 and a secondary collection tube 14. The primary collection tube 12 is formed of a quartz tubular body, and a gas supply plug 16 that is an air flow inlet is attached to the upper end opening, and a test piece container 20 that can accommodate a test piece 18 in the upstream part. It is said. A lower area of the test piece container 20 is an organic volatiles adsorption unit 22. An airflow guide member 24 that guides the airflow passing through the adsorption portion 22 to the inner wall of the pipe is disposed in the adsorption portion 22. The airflow guide member 24 has a structure in which a quartz plate 24B is fixed as an airflow blocking member at a central portion of a quartz filter 24A arranged so as to block the cross section of the tube, and an annular shape is provided between the side portion of the quartz plate 24B and the inner wall of the tube. A gap S is formed. The airflow passing through the adsorption part passes through the annular gap S avoiding the quartz plate 24B, and as a result, the airflow is guided to the inner wall of the tube. Below the airflow guide member 24 is a tapered tapered portion 26, and a connecting portion 28 is formed at the lower end of the tapered portion 26.

二次捕集管14も一次捕集管12と同様に石英製の管状体で形成され、上端に連結部30が形成されている。この連結部30と一次捕集管12の連結部28とをコネクタ32によって連結することにより、一次捕集管12と二次捕集管14は連通する。二次捕集管14内には石英フィルタ34が取り付けられている。石英フィルタ34の下方エリアが有機揮発物の捕集剤充填部36とされ、例えば多孔性ポリマー吸着剤(商品名:テナックス)などの捕集剤が充填されている。捕集剤充填部36の下端側には石英ウール38が詰め込まれており、前記捕集剤を固定して捕集剤が下方に落下することを防いでいる。二次捕集管14の下端開口にはガス排出栓40が取り付けられており、このガス排出栓40が気流の流出口とされる。一次捕集管12と二次捕集管14とは、コネクタ32を取り外すことによって切り離し可能とされる。切り離した一次捕集管12及び二次捕集管14のそれぞれが単独で熱脱着型ガスクロマトグラフ装置の熱脱着部に装填可能とされる。   Similarly to the primary collection tube 12, the secondary collection tube 14 is also formed of a quartz tubular body, and a connecting portion 30 is formed at the upper end. By connecting the connecting portion 30 and the connecting portion 28 of the primary collection tube 12 with a connector 32, the primary collection tube 12 and the secondary collection tube 14 communicate with each other. A quartz filter 34 is attached in the secondary collection tube 14. A lower area of the quartz filter 34 is an organic volatile trapping agent filling section 36, and is filled with a trapping agent such as a porous polymer adsorbent (trade name: Tenax). Quartz wool 38 is packed in the lower end side of the collecting agent filling portion 36 to fix the collecting agent and prevent the collecting agent from falling downward. A gas discharge plug 40 is attached to the lower end opening of the secondary collection pipe 14, and this gas discharge plug 40 serves as an airflow outlet. The primary collection tube 12 and the secondary collection tube 14 can be separated by removing the connector 32. Each of the separated primary collection pipe 12 and secondary collection pipe 14 can be independently loaded into the thermal desorption section of the thermal desorption type gas chromatograph apparatus.

以下、上記の捕集管10を用いた有機揮発物の測定方法を図2に基づいて説明する。まず、測定前の予備処理として一次捕集管12と二次捕集管14を切り離した状態で、それぞれの加熱清浄処理を別個に行う(S100)。一次捕集管12の加熱清浄処理は、試験片収容部20に試験片18を収容しない空の状態で管内に高純度窒素を流しつつ、280℃で1時間、加熱する。この加熱によって管内壁や石英フィルタ24A、石英板24Bに吸着している有機揮発物が揮発し、一次捕集管12内が浄化される。二次捕集管14の加熱清浄処理も同様に管内に高純度窒素を流しつつ、280℃で3時間、加熱し、捕集剤充填部36の捕集剤などに吸着している有機揮発物を揮発させ排出する。加熱時間を3時間と長くする理由は有機揮発物に対する捕集剤の吸着力が強いので、有機揮発物を完全に脱着させるために時間を要するからである。次のS110で一次捕集管12と二次捕集管14とをコネクタ32を用いて連結する。なお、このS100とS110では上記の手順とは逆に一次捕集管12と二次捕集管14を連結した状態で一次捕集管12のガス供給栓16又は二次捕集管14のガス排出栓40のいずれか一方から高純度窒素を流して、一次捕集管12と二次捕集管14を同時に加熱清浄処理するようにしてもよい。   Hereinafter, a method for measuring organic volatiles using the collection tube 10 will be described with reference to FIG. First, each heat cleaning process is performed separately in the state which separated the primary collection pipe | tube 12 and the secondary collection pipe | tube 14 as a preliminary | backup process before a measurement (S100). The heating and cleaning process of the primary collection tube 12 is performed at 280 ° C. for 1 hour while flowing high-purity nitrogen into the tube in an empty state where the test piece 18 is not accommodated in the test piece accommodation unit 20. By this heating, organic volatiles adsorbed on the inner wall of the tube, the quartz filter 24A, and the quartz plate 24B are volatilized, and the inside of the primary collection tube 12 is purified. Similarly, the heating and cleaning treatment of the secondary collection tube 14 is heated at 280 ° C. for 3 hours while flowing high-purity nitrogen in the tube, and is adsorbed on the collection agent or the like of the collection agent filling unit 36. Volatilize and discharge. The reason why the heating time is increased to 3 hours is that it takes time to completely desorb the organic volatiles because the adsorbing power of the scavenger to the organic volatiles is strong. In next S 110, the primary collection tube 12 and the secondary collection tube 14 are connected using the connector 32. In S100 and S110, the gas of the gas supply plug 16 of the primary collection pipe 12 or the gas of the secondary collection pipe 14 in a state in which the primary collection pipe 12 and the secondary collection pipe 14 are connected in reverse to the above procedure. High purity nitrogen may be flowed from either one of the discharge plugs 40 to heat and clean the primary collection pipe 12 and the secondary collection pipe 14 simultaneously.

S120では試験片18の予備処理を行う。試験片18は測定対象である有機材料などを一次捕集管12の試験片収容部20に収容可能な寸法に加工したものである。予備処理ではこの試験片18を空気に暴露する。暴露用の空気としては有機物などの不純物を除去した清浄空気を用いる。また、暴露時間は例えば48時間程度とする。この予備処理は試験片18を測定対象である材料が例えばクリーンルームの構成材として実際に使用される時と同じ状態にすることを目的としている。したがって、測定対象である材料が実際に使用される状態を勘案して予備処理での暴露条件を適宜、設定することになる。   In S120, the test piece 18 is preliminarily processed. The test piece 18 is obtained by processing an organic material or the like to be measured into a size that can be accommodated in the test piece accommodation portion 20 of the primary collection tube 12. In the pretreatment, the test piece 18 is exposed to air. As the air for exposure, clean air from which impurities such as organic substances have been removed is used. The exposure time is about 48 hours, for example. The purpose of this pretreatment is to make the test piece 18 in the same state as when the material to be measured is actually used as, for example, a clean room component. Therefore, the exposure conditions in the pretreatment are appropriately set in consideration of the state in which the material to be measured is actually used.

S130では上記予備処理が終了した試験片18を一次捕集管12の試験片収容部20に装着する。図1には試験片18を装着した状態が示されている。すなわち、一次捕集管12をガス供給栓16が上方に位置するように鉛直に配置し、試験片18を径が0.1mm程度のステンレス細線42を用いてガス供給栓16から吊り下げる。   In S <b> 130, the test piece 18 for which the preliminary processing has been completed is attached to the test piece storage unit 20 of the primary collection tube 12. FIG. 1 shows a state in which the test piece 18 is mounted. That is, the primary collection pipe 12 is vertically arranged so that the gas supply plug 16 is positioned above, and the test piece 18 is suspended from the gas supply plug 16 using a stainless steel wire 42 having a diameter of about 0.1 mm.

S140ではサンプリングを行う。このサンプリングは図1に示したように試験片18を一次捕集管12の試験片収容部20に中吊とし、試験片18が管内壁に接触しない状態で、ガス供給栓16から空気を流すことによって行う。サンプリング用の空気としては有機物などを活性炭によって除去した清浄空気を所定の温湿度に調整したものを用いる。また、供給空気量は管内の空気流速が0.1〜2.0m/秒となるようにする。サンプリング時間は25〜320分の範囲とする。このサンプリングによって試験片18に含まれる有機揮発物が試験片18の表面から継続的に揮発する。揮発した有機揮発物のうち、吸着性が強いものは図3に示したように主に一次捕集管12の吸着部22の管内壁や下部の石英フィルタ24Aと石英板24Bに吸着する。一方、吸着性が弱い有機揮発物は一次捕集管12を通り抜けて、主に二次捕集管14の捕集剤充填部36で捕集される。すなわち、捕集剤充填部36に充填された多孔性ポリマー吸着剤(商品名:テナックス)は有機揮発物に対する吸着力が大きい捕集剤であり、吸着性が弱い低濃度の有機揮発物であってもその吸着力によって確実に捕集する。なお、試験片18を吊るステンレス細線42からも微量の有機揮発物が揮発する恐れがあるが、ステンレス細線42の表面積は試験片18の表面積に比べて著しく小さいので、その影響は無視できる。   In S140, sampling is performed. In this sampling, as shown in FIG. 1, the test piece 18 is suspended from the test piece housing portion 20 of the primary collection tube 12, and air is allowed to flow from the gas supply plug 16 without the test piece 18 being in contact with the inner wall of the tube. By doing. As sampling air, use is made of clean air obtained by removing organic substances or the like with activated carbon and adjusted to a predetermined temperature and humidity. The supply air amount is set so that the air flow rate in the pipe is 0.1 to 2.0 m / sec. The sampling time is in the range of 25 to 320 minutes. By this sampling, the organic volatiles contained in the test piece 18 are continuously volatilized from the surface of the test piece 18. Among the volatilized organic volatiles, those having strong adsorptivity are mainly adsorbed on the inner wall of the adsorbing portion 22 of the primary collection tube 12 and the lower quartz filter 24A and the quartz plate 24B as shown in FIG. On the other hand, organic volatiles having a weak adsorptivity pass through the primary collection tube 12 and are collected mainly by the collection agent filling section 36 of the secondary collection tube 14. That is, the porous polymer adsorbent (trade name: Tenax) filled in the collector filling portion 36 is a collector having a large adsorbing power for organic volatiles, and is a low concentration organic volatile having a low adsorbability. However, it is reliably collected by its adsorption power. Although a small amount of organic volatiles may be volatilized from the stainless steel wire 42 that suspends the test piece 18, the surface area of the stainless steel wire 42 is remarkably smaller than the surface area of the test piece 18, so the influence can be ignored.

S140のサンプリングが終了すると次のS150の測定・分析に移る。測定・分析には熱脱着型ガスクロマトグラフ装置を用い、一次捕集管12と二次捕集管14について別個に測定・分析する。サンプリングが終了した捕集管10を一次捕集管12と二次捕集管14に切り離し、一次捕集管12については試験片18を抜き出した後に熱脱着型ガスクロマトグラフ装置にかける。図4は熱脱着型ガスクロマトグラフ装置の模式図である。当該装置50は熱脱着部52、ガスクロマトグラフ54、質量分析部56とからなり、熱脱着部52に前記の一次捕集管12又は二次捕集管14を装填することによって、それぞれの捕集管に捕集された有機揮発物の種類と量を測定・分析する。   When the sampling of S140 is completed, the process proceeds to the next measurement / analysis of S150. For the measurement and analysis, a thermal desorption type gas chromatograph apparatus is used, and the primary collection tube 12 and the secondary collection tube 14 are separately measured and analyzed. The sampling tube 10 for which sampling has been completed is separated into a primary collection tube 12 and a secondary collection tube 14, and the test piece 18 is extracted from the primary collection tube 12 and then applied to a thermal desorption type gas chromatograph apparatus. FIG. 4 is a schematic diagram of a thermal desorption type gas chromatograph apparatus. The apparatus 50 includes a thermal desorption unit 52, a gas chromatograph 54, and a mass analysis unit 56. By loading the primary collection tube 12 or the secondary collection tube 14 into the thermal desorption unit 52, the respective collections are performed. Measure and analyze the type and amount of organic volatiles collected in the tube.

すなわち、熱脱着部52では装填した捕集管12(又は14)にガスボンベ58からキャリアガスを流しながら、捕集管12(又は14)をヒータ59によって所定の温度に加熱する。すると、捕集管12(又は14)に吸着されていた有機揮発物が捕集管12(又は14)の各部位から脱着し、ガスクロマトグラフ54に送られる。ガスクロマトグラフ54では複数種の有機揮発物がそれぞれの吸着性によって移動速度に差異を生じて展開・分離され、時間差を有して質量分析部56に到達する。したがって、質量分析部56では有機揮発物の種類ごとにその量を検出することができる。   That is, the thermal desorption section 52 heats the collection tube 12 (or 14) to a predetermined temperature by the heater 59 while flowing the carrier gas from the gas cylinder 58 to the loaded collection tube 12 (or 14). Then, the organic volatile matter adsorbed on the collection tube 12 (or 14) is desorbed from each part of the collection tube 12 (or 14) and sent to the gas chromatograph 54. In the gas chromatograph 54, a plurality of types of organic volatiles are developed and separated with a difference in moving speed due to their adsorptivity, and reach the mass spectrometer 56 with a time difference. Therefore, the mass analyzer 56 can detect the amount of each type of organic volatile matter.

図5は一次捕集管が熱脱着部52で熱脱着を受ける際のキャリアガスの流れ状況を示した説明図であり、(1)は本発明に係る一次捕集管12の場合、(2)は本発明外の一次捕集管60の場合を示す。図5(1)に示した本発明に係る一次捕集管12では吸着部22には石英フィルタ24Aと石英板24Bからなる気流案内部材24が配置されている。このため吸着部22を通過するキャリアガスCは石英板24Bを避けて環状の隙間Sを通ることになり、キャリアガスCは管内壁に案内される。したがって、キャリアガスCは管内壁に吸着している有機揮発物と十分に接触し、有機揮発物を確実に脱着させる。このため、有機揮発物の脱着率を高くすることができ、熱脱着型ガスクロマトグラフ装置50の測定精度を向上させる。一方、図5(2)に示した気流案内部材を有しない本発明外の一次捕集管60では、キャリアガスCが管中心部に流れ易い。このため、キャリアガスCと管内壁に吸着している有機揮発物との接触が不十分となり、有機揮発物の脱着が不確実になる。したがって、有機揮発物の脱着率が低くなり、熱脱着型ガスクロマトグラフ装置50の測定精度が低下する。   FIG. 5 is an explanatory view showing the flow state of the carrier gas when the primary collection tube is subjected to thermal desorption at the thermal desorption section 52. (1) is the case of the primary collection tube 12 according to the present invention, (2 ) Shows the case of the primary collection tube 60 outside the present invention. In the primary collection tube 12 according to the present invention shown in FIG. 5 (1), an airflow guide member 24 composed of a quartz filter 24 A and a quartz plate 24 B is disposed in the adsorption portion 22. For this reason, the carrier gas C passing through the adsorbing portion 22 passes through the annular gap S avoiding the quartz plate 24B, and the carrier gas C is guided to the inner wall of the pipe. Therefore, the carrier gas C is sufficiently in contact with the organic volatiles adsorbed on the inner wall of the pipe and reliably desorbs the organic volatiles. For this reason, the desorption rate of organic volatiles can be increased, and the measurement accuracy of the thermal desorption type gas chromatograph apparatus 50 is improved. On the other hand, in the primary collection pipe 60 outside the present invention that does not have the airflow guide member shown in FIG. 5 (2), the carrier gas C is easy to flow to the pipe center. For this reason, the contact between the carrier gas C and the organic volatile matter adsorbed on the inner wall of the pipe becomes insufficient, and the desorption of the organic volatile matter becomes uncertain. Therefore, the desorption rate of organic volatiles is lowered, and the measurement accuracy of the thermal desorption type gas chromatograph apparatus 50 is lowered.

図6は図5(1)に示した本発明に係る一次捕集管12を用いた場合の熱脱着型ガスクロマトグラフ装置50での質量分析結果を例示したスペクトル図である。一次捕集管での検出において、保持時間25分で検出された有機揮発物は吸着性の強いジオクチルフタル酸(DOP)である。二次捕集管ではDOPは検出されていない。このことから、サンプリング時に使用した試験片からはDOPが盛んに揮発していること、及び揮発したDOPのほぼ全量が石英フィルタ24Aと石英板24Bを含む吸着部22に吸着・捕集され、二次捕集管14には到達しなかったことを如実に示している。   FIG. 6 is a spectrum diagram illustrating the results of mass spectrometry in the thermal desorption type gas chromatograph apparatus 50 when the primary collection tube 12 according to the present invention shown in FIG. In the detection by the primary collection tube, the organic volatile matter detected at a retention time of 25 minutes is dioctylphthalic acid (DOP) having strong adsorptivity. DOP is not detected in the secondary collection tube. From this, DOP is actively volatilized from the test piece used at the time of sampling, and almost all of the volatilized DOP is adsorbed and collected by the adsorption unit 22 including the quartz filter 24A and the quartz plate 24B. It clearly shows that the next collection tube 14 has not been reached.

図7は図5(2)に示した本発明外の一次捕集管60を用いた場合の熱脱着型ガスクロマトグラフ装置50での質量分析結果を例示したスペクトル図である。サンプリング条件は図6に示した条件と同一である。この場合でも図6に示した結果と同様の傾向がある。しかしながら、一次捕集管での検出において、保持時間25分で検出されたDOPの量が半分程度に低下している。このことから、本発明外の一次捕集管60を用いた場合には、熱脱着型ガスクロマトグラフ装置50の熱脱着部52でのDOPの脱着が不十分であるため、DOPの質量分析値が小さくなること及び測定繰り返し再現性が悪くなることを示している。   FIG. 7 is a spectrum diagram illustrating the results of mass spectrometry in the thermal desorption type gas chromatograph apparatus 50 when the primary collection tube 60 outside the present invention shown in FIG. 5 (2) is used. Sampling conditions are the same as those shown in FIG. Even in this case, there is a tendency similar to the result shown in FIG. However, in the detection with the primary collection tube, the amount of DOP detected in the holding time of 25 minutes is reduced to about half. From this, when the primary collection tube 60 outside the present invention is used, since the desorption of DOP in the thermal desorption section 52 of the thermal desorption gas chromatograph apparatus 50 is insufficient, the mass spectrometric value of DOP is It shows that it becomes smaller and the repeatability of measurement repeats worsens.

上述のとおり、本実施形態の有機揮発物測定用捕集管10は、一次捕集管12と二次捕集管14に分割されており、一次捕集管12には試験片収容部20と吸着部22とが配置されている。また、二次捕集管14には捕集剤充填部36が配置されている。したがって、サンプリング時には両者を連結して使用し、測定・分析時には両者を切り離して一次捕集管12及び二次捕集管14をそれぞれ単独で熱脱着型ガスクロマトグラフ装置50の熱脱着部52に装填して測定・分析を行うことができる。このため、試験片18から揮発する有機揮発物の種類、量のみならず、揮発した有機揮発物の吸着性に関する傾向を究明する場合に有効である。また、一次捕集管12には気流案内部材24が配置されており、吸着部22を通過する気流を管内壁に案内するようにしている。このため、一次捕集管12を熱脱着型ガスクロマトグラフ装置50の熱脱着部52に装填して熱脱着を行う際には、キャリアガスが管内壁に吸着している有機揮発物と十分に接触し、有機揮発物を確実に脱着させる。このため、有機揮発物の脱着率を高くすることができ、熱脱着型ガスクロマトグラフ装置50での測定精度を向上させることができる。   As described above, the organic volatile matter measuring collection tube 10 of the present embodiment is divided into a primary collection tube 12 and a secondary collection tube 14, and the primary collection tube 12 includes a test piece container 20 and A suction part 22 is arranged. Further, a collection agent filling portion 36 is disposed in the secondary collection tube 14. Therefore, the two are connected and used at the time of sampling, and both are separated at the time of measurement / analysis, and the primary collection tube 12 and the secondary collection tube 14 are each loaded in the thermal desorption section 52 of the thermal desorption type gas chromatograph apparatus 50 alone. Can be measured and analyzed. For this reason, it is effective when investigating the tendency regarding not only the kind and amount of organic volatiles that volatilize from the test piece 18 but also the adsorptivity of the volatile organic volatiles. Further, an air flow guide member 24 is disposed in the primary collection tube 12 so as to guide the air flow passing through the adsorption portion 22 to the inner wall of the tube. For this reason, when the primary collection tube 12 is loaded into the thermal desorption section 52 of the thermal desorption type gas chromatograph apparatus 50 and thermal desorption is performed, the carrier gas sufficiently contacts the organic volatiles adsorbed on the inner wall of the tube. And ensure that organic volatiles are desorbed. For this reason, the desorption rate of organic volatiles can be increased, and the measurement accuracy in the thermal desorption type gas chromatograph apparatus 50 can be improved.

図8は一次捕集管12に配置する気流案内部材の変形例を示す断面図である。図8(1)は気流遮断部材である石英板24Bが管中央に位置するように支持材24Dによって支持した例である。図8(2)は(1)と同様の石英板24Bの下方に石英ウール24Eを配置した例である。図8(3)は環状の石英フィルタ24Fの中央部に石英板24Bを埋め込み、一体化したものを管内壁に融着した例である。(2)(3)に示したものはサンプリング時には石英ウール24Eや石英フィルタ24Fが吸着性の強い有機揮発物を捕集する上で補助的な役割を果たす。   FIG. 8 is a cross-sectional view showing a modified example of the airflow guide member disposed in the primary collection tube 12. FIG. 8A shows an example in which the quartz plate 24B, which is an airflow blocking member, is supported by the support member 24D so as to be located at the center of the tube. FIG. 8B is an example in which quartz wool 24E is disposed below a quartz plate 24B similar to (1). FIG. 8 (3) shows an example in which a quartz plate 24B is embedded in the center of an annular quartz filter 24F, and an integrated one is fused to the inner wall of the tube. (2) In the case shown in (3), the quartz wool 24E and the quartz filter 24F play an auxiliary role in collecting strongly adsorbing organic volatiles during sampling.

図9は本発明に係る有機揮発物測定用捕集管の第2実施形態を示す断面図である。当該捕集管70は管状体で形成され、上端開口に気流の流入口であるガス供給栓72が取り付けられる。そして、気流の上流側から順次、試験片18を収容可能な試験片収容部73、有機揮発物の吸着部74と、この吸着部74を通過する気流を管内壁に案内する気流案内部材76と、有機揮発物の捕集剤充填部78が配置されている。下端開口には気流の流出口であるガス排出栓80が取り付けられる。   FIG. 9 is a sectional view showing a second embodiment of the organic volatile matter measuring collection tube according to the present invention. The collection tube 70 is formed of a tubular body, and a gas supply plug 72 as an airflow inlet is attached to the upper end opening. And, sequentially from the upstream side of the air flow, a test piece housing part 73 capable of housing the test piece 18, an organic volatile matter adsorption part 74, and an air flow guide member 76 for guiding the air flow passing through the adsorption part 74 to the inner wall of the pipe An organic volatile scavenger filling unit 78 is disposed. A gas discharge plug 80 which is an outlet for airflow is attached to the lower end opening.

この捕集管70を用いて有機揮発物を測定する場合にも、図2に示した手順と同様の方法で、サンプリングと測定・分析を行う。ただし、捕集管70は第1実施形態のように分割されていないので、図2におけるS110の連結操作は不要である。この捕集管70にも気流案内部材76が配置されており、吸着部74を通過する気流を管内壁に案内するようにしている。したがって、サンプリング終了後の捕集管70を熱脱着型ガスクロマトグラフ装置の熱脱着部に装填して熱脱着を行う際には、キャリアガスが管内壁に吸着している有機揮発物と十分に接触し、有機揮発物を確実に脱着させる。このため、有機揮発物の脱着率を高くすることができ、熱脱着型ガスクロマトグラフ装置での測定精度を向上させることができる。なお、捕集管70を熱脱着部に装填する際には装填方向を逆向きとし、熱脱着時にキャリアガスがガス排出栓80側から流入し、ガス供給栓72から抜けるようにすることが好ましい。このように装填することによって、吸着力が強い捕集剤充填部78の捕集剤から脱着した有機揮発物が再吸着を繰り返すことなくキャリアガスに円滑に運ばれるので、熱脱着操作を効率よく行うことができ、測定精度を向上させることができる。   Even when organic volatiles are measured using the collection tube 70, sampling, measurement, and analysis are performed in the same manner as the procedure shown in FIG. However, since the collection tube 70 is not divided as in the first embodiment, the connecting operation of S110 in FIG. 2 is not necessary. An airflow guide member 76 is also disposed in the collecting pipe 70 so as to guide the airflow passing through the adsorption portion 74 to the inner wall of the pipe. Therefore, when the sampling tube 70 after sampling is loaded into the thermal desorption section of the thermal desorption type gas chromatograph and thermal desorption is performed, the carrier gas is in sufficient contact with the organic volatiles adsorbed on the inner wall of the tube. And ensure that organic volatiles are desorbed. For this reason, the desorption rate of the organic volatile matter can be increased, and the measurement accuracy in the thermal desorption type gas chromatograph apparatus can be improved. When loading the collection tube 70 into the thermal desorption section, it is preferable to reverse the loading direction so that the carrier gas flows from the gas discharge plug 80 side and escapes from the gas supply plug 72 during the thermal desorption. . By loading in this manner, the organic volatiles desorbed from the collecting agent of the collecting agent filling section 78 having a strong adsorbing force are smoothly carried to the carrier gas without repeating re-adsorption, so that the thermal desorption operation is efficiently performed. Measurement accuracy can be improved.

上記実施形態では捕集管を構成する各部の材料が主に石英である場合について説明した。しかしながら、本発明はこれに限らず、捕集管を構成する各部の材料として他の材質のものを用いるようにしてもよい。例えば、シリコン系ウエハに対する有機揮発物の付着状況を調べたい場合には、捕集管を構成する各部の材料としてシリコン系のものを用いることが望ましい。調査対象品が金属やガラスである場合にも、捕集管を構成する各部の材料として同材質のものを選択することが望ましい。   In the above embodiment, the case where the material of each part constituting the collection tube is mainly quartz has been described. However, the present invention is not limited to this, and other materials may be used as the material of each part constituting the collection tube. For example, when it is desired to examine the state of adhesion of organic volatiles to a silicon-based wafer, it is desirable to use a silicon-based material as the material of each part constituting the collection tube. Even when the investigation object is a metal or glass, it is desirable to select the same material as the material of each part constituting the collection tube.

上記実施形態では熱脱着型ガスクロマトグラフ装置として、質量分析部を備えたものを説明した。しかしながら、本発明に係る熱脱着型ガスクロマトグラフ装置はこれに限らず、質量分析部に代わる各種の分析部を備えたものを用いることができる。   In the said embodiment, what was provided with the mass-analysis part was demonstrated as a thermal desorption type gas chromatograph apparatus. However, the thermal desorption type gas chromatograph apparatus according to the present invention is not limited to this, and an apparatus equipped with various analysis units instead of the mass analysis unit can be used.

本発明に係る有機揮発物測定用捕集管の第1実施形態を示す断面図である。It is sectional drawing which shows 1st Embodiment of the collection tube for organic volatile matter measurement which concerns on this invention. 本発明に係る有機揮発物測定方法の測定手順を示す説明図である。It is explanatory drawing which shows the measurement procedure of the organic volatile matter measuring method which concerns on this invention. 一次捕集管の吸着部における有機揮発物の吸着状況を示す説明図である。It is explanatory drawing which shows the adsorption | suction state of the organic volatile matter in the adsorption | suction part of a primary collection tube. 熱脱着型ガスクロマトグラフ装置の模式図である。It is a schematic diagram of a thermal desorption type gas chromatograph apparatus. 一次捕集管が熱脱着部で熱脱着を受ける際のキャリアガスの流れ状況を示した説明図である。It is explanatory drawing which showed the flow condition of the carrier gas at the time of a primary collection pipe receiving thermal desorption in a thermal desorption part. 本発明に係る一次捕集管を用いた場合の熱脱着型ガスクロマトグラフ装置での質量分析結果を例示したスペクトル図である。It is the spectrum figure which illustrated the mass spectrometry result in the thermal desorption type gas chromatograph device at the time of using the primary collection tube concerning the present invention. 本発明外の一次捕集管を用いた場合の熱脱着型ガスクロマトグラフ装置での質量分析結果を例示したスペクトル図である。It is the spectrum figure which illustrated the mass spectrometry result in the thermal desorption type gas chromatograph device at the time of using the primary collection tube outside the present invention. 一次捕集管に配置する気流案内部材の変形例を示す断面図である。It is sectional drawing which shows the modification of the airflow guide member arrange | positioned at a primary collection pipe. 本発明に係る有機揮発物測定用捕集管の第2実施形態を示す断面図である。It is sectional drawing which shows 2nd Embodiment of the collection tube for organic volatile matter measurement which concerns on this invention. 従来技術に係る有機揮発物測定方法を示す概要図である。It is a schematic diagram which shows the organic volatile matter measuring method which concerns on a prior art.

符号の説明Explanation of symbols

10………捕集管、12………一次捕集管、14………二次捕集管、16………ガス供給栓、18………試験片、20………試験片収容部、22………吸着部、24………気流案内部材、24A………石英フィルタ、24B………石英板、28,30………連結部、32………コネクタ、34………石英フィルタ、36………捕集剤充填部、38………石英ウール、40………ガス排出栓、50………熱脱着型ガスクロマトグラフ装置、52………熱脱着部、54………ガスクロマトグラフ、56………質量分析部、60………(本発明外の)一次捕集管、70………捕集管、72………ガス供給栓、73………試験片収容部、74………吸着部、76………気流案内部材、78………捕集剤充填部、80………ガス排出栓。

10 ......... Collecting tube, 12 ......... Primary collecting tube, 14 ......... Secondary collecting tube, 16 ...... Gas supply plug, 18 ......... Test specimen, 20 ......... Test specimen container , 22 ......... Adsorption part, 24 ... ... Airflow guide member, 24A ... ... Quartz filter, 24B ... ... Quartz plate, 28, 30 ... ... Connection part, 32 ... ... Connector, 34 ... ... Quartz Filter, 36 ......... Filling agent filling section, 38 ......... Quartz wool, 40 ......... Gas discharge plug, 50 ......... Heat desorption type gas chromatograph, 52 ......... Heat desorption section, 54 ......... Gas chromatograph, 56... Mass spectrometer, 60... Primary collection tube (outside of the present invention) 70... Collection tube, 72... Gas supply plug, 73. 74 ......... Adsorption part, 76 ...... Airflow guide member, 78 ......... Filling agent filling part, 80 ...... Gas discharge plug.

Claims (4)

気流の流入口と流出口を備えた管状体と、この管状体の上流部に配置されて試験片を収容可能な試験片収容部と、前記管状体の下流部に配置された有機揮発物の捕集剤充填部と、前記試験片収容部と捕集剤充填部との中間に配置された有機揮発物の吸着部と、当該吸着部を通過する気流を管内壁に案内する気流案内部材とを具備し、熱脱着型ガスクロマトグラフ装置の熱脱着部に直接に装填可能とされたことを特徴とする有機揮発物測定用捕集管。   A tubular body having an airflow inlet and an outlet, a test piece container disposed in an upstream portion of the tubular body and capable of accommodating a test piece, and an organic volatile substance disposed in a downstream portion of the tubular body. A collector filling portion, an organic volatiles adsorbing portion disposed between the test piece container and the collecting agent filling portion, and an airflow guide member for guiding the airflow passing through the adsorbing portion to the inner wall of the pipe; A collection tube for measuring organic volatile matter, characterized in that it can be directly loaded into a thermal desorption part of a thermal desorption type gas chromatograph apparatus. 前記有機揮発物測定用捕集管が一次捕集管と二次捕集管に分割されており、一次捕集管には前記試験片収容部と前記吸着部と前記気流案内部材とが配置され、二次捕集管には前記捕集剤充填部が配置され、前記一次捕集管及び二次捕集管がそれぞれ単独で熱脱着型ガスクロマトグラフ装置の熱脱着部に装填可能とされたことを特徴とする請求項1に記載の有機揮発物測定用捕集管。   The organic volatile matter measuring collection tube is divided into a primary collection tube and a secondary collection tube, and the test piece storage unit, the adsorption unit, and the airflow guide member are arranged in the primary collection tube. The secondary collection tube is provided with the collecting agent filling unit, and the primary collection tube and the secondary collection tube can each be independently loaded into the thermal desorption unit of the thermal desorption type gas chromatograph apparatus. The collection tube for measuring organic volatile matter according to claim 1. 前記気流案内部材がフィルタ部材の中央部に気流遮断部材を配した構成とされ、管断面に対して前記気流を環状に案内することを特徴とする請求項1又は請求項2に記載の有機揮発物測定用捕集管。   3. The organic volatilization according to claim 1, wherein the air flow guide member has a structure in which an air flow blocking member is disposed in a central portion of the filter member, and guides the air flow in an annular shape with respect to a pipe cross section. Collection tube for measuring objects. 請求項1乃至請求項3のいずれかに記載された前記捕集管を気流の流入口が上方に位置するように鉛直に配置し、前記試験片を前記流入口から吊り下げた状態で前記捕集管に収容し、当該捕集管内に空気を導入して前記試験片から揮発した有機揮発物を前記吸着部及び捕集剤充填部で吸着、捕集する第1工程と、第1工程後の捕集管から前記試験片を抜き出した後に、当該捕集管を熱脱着型ガスクロマトグラフ装置の熱脱着部に装填し、前記捕集管に吸着、捕集された有機揮発物を前記熱脱着型ガスクロマトグラフ装置によって分析する第2工程とを含むことを特徴とする有機揮発物測定方法。

The collecting pipe according to any one of claims 1 to 3 is arranged vertically so that an airflow inlet is located above, and the test piece is suspended from the inlet and the trapping is performed. A first step in which the organic volatiles contained in the collecting tube, air is introduced into the collecting tube, and volatilized from the test piece are adsorbed and collected by the adsorbing unit and the collecting agent filling unit, and after the first step After extracting the test piece from the collection tube, the collection tube is loaded into a thermal desorption section of a thermal desorption type gas chromatograph device, and the organic volatiles adsorbed and collected in the collection tube are desorbed in the heat. The organic volatile matter measuring method characterized by including the 2nd process analyzed by a type | mold gas chromatograph apparatus.

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