JPH03197834A - Method for measuring evaporation of organic solvent and pretreating device for measurement of evaporation - Google Patents
Method for measuring evaporation of organic solvent and pretreating device for measurement of evaporationInfo
- Publication number
- JPH03197834A JPH03197834A JP33759289A JP33759289A JPH03197834A JP H03197834 A JPH03197834 A JP H03197834A JP 33759289 A JP33759289 A JP 33759289A JP 33759289 A JP33759289 A JP 33759289A JP H03197834 A JPH03197834 A JP H03197834A
- Authority
- JP
- Japan
- Prior art keywords
- organic solvent
- bottle
- heating container
- gas
- vacuum bottle
- 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
- 238000005259 measurement Methods 0.000 title claims abstract description 27
- 239000003960 organic solvent Substances 0.000 title claims description 28
- 238000000034 method Methods 0.000 title description 13
- 230000008020 evaporation Effects 0.000 title 2
- 238000001704 evaporation Methods 0.000 title 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 239000007789 gas Substances 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000009834 vaporization Methods 0.000 claims description 12
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 9
- 230000008016 vaporization Effects 0.000 claims description 9
- 238000000691 measurement method Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000002689 soil Substances 0.000 abstract description 7
- 239000001307 helium Substances 0.000 abstract description 2
- 229910052734 helium Inorganic materials 0.000 abstract description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 238000000638 solvent extraction Methods 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000004045 organic chlorine compounds Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000011364 vaporized material Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野］
本発明は化学分析用試料の前処理方法及び前処理器に関
し、特に固体試料中に吸収あるいは吸着している有機溶
剤を高感度で迅速に測定するための試料の前処理方法及
び前処理装置に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a pretreatment method and a pretreatment device for samples for chemical analysis, and in particular to a method for rapidly and highly sensitively removing organic solvents absorbed or adsorbed in solid samples. The present invention relates to a sample pretreatment method and pretreatment device for measurement.
［従来の技術］
従来、土壌、活性炭、汚泥等の固形試料に取り込まれて
いる有機塩素化合物等の有機溶剤の分析に際し、あらか
じめ行われる前処理について、例えば、溶媒抽呂法は、
土壌、活性炭に、試料の１〜１０倍量のｎ−ヘキサンあ
るいは二硫化炭素等の抽出溶媒を加えて密封し、混合振
り混ぜた後、定時間放置して測定成分を抽出する前処理
を行い、この抽出液についてガスクロマトグラフ分析等
を行うものである。[Prior Art] Conventionally, when analyzing organic solvents such as organic chlorine compounds incorporated in solid samples such as soil, activated carbon, and sludge, pretreatments performed in advance include, for example, the solvent extraction method.
Add an extraction solvent such as n-hexane or carbon disulfide in an amount 1 to 10 times the amount of the sample to the soil or activated carbon, seal it, shake it, and then leave it for a certain period of time for pretreatment to extract the components to be measured. This extract is subjected to gas chromatography analysis and the like.
また、加熱気化法は、土壌、活性炭等の測定しようとす
る試料の一定量を測定系のキャリアガス流路系の前段に
直接組み込まれている加熱部に挿入し、測定成分を気化
し、この気化ガスをキャリアガスと共にガスクロマトグ
ラフ等の測定系に送り、分析測定を行うものである。In addition, in the thermal vaporization method, a certain amount of the sample to be measured, such as soil or activated carbon, is inserted into a heating section that is built directly into the front stage of the carrier gas flow path system of the measurement system, and the component to be measured is vaporized. The vaporized gas is sent together with a carrier gas to a measurement system such as a gas chromatograph for analysis and measurement.
［発明が解決しようとする課題］
上述した従来の溶媒抽出法では、■特に水分を含む土壌
等の場合、抽出用有機溶媒と混合振とうしても、十分な
量が抽出されるまでは、試料により１０日以上も浸漬す
る必要がある場合があり、長時間を要すること、■試料
により懸濁し、溶媒層と試料層が分離しにくいこと、■
測定目的以外の高沸点成分も同時に抽出され、これが測
定機器を汚染してしまうこと、■抽出用溶媒は一般に引
火点が低く、また人体にも有害で、危険性が高いこと等
の欠点があった。また、従来の加熱気化法では、■注入
時のサンプルガス容積が大きくなるため、ガスクロマト
グラフ測定法などでクロマト分離する際、分離性が悪く
、クロマトグラムの各ピークもブロードで感度も低下し
てしまうこと１．２１回の試料使用量、が少なく試料全
体に対して、得られたデータに９遍性がないこと等の欠
点があった。[Problems to be Solved by the Invention] In the conventional solvent extraction method described above, ■ Especially in the case of soil containing moisture, even if mixed with an organic solvent for extraction and shaken, until a sufficient amount is extracted, Depending on the sample, it may be necessary to immerse it for more than 10 days, which takes a long time; ■ Depending on the sample, the sample may be suspended, making it difficult to separate the solvent layer and the sample layer; ■
High boiling point components other than those intended for measurement are also extracted at the same time, which contaminates the measuring equipment. Extraction solvents generally have low flash points and are harmful to the human body, making them highly dangerous. Ta. In addition, in the conventional thermal vaporization method, ■The sample gas volume during injection is large, so when performing chromatographic separation using gas chromatography measurement methods, separation performance is poor, and each peak in the chromatogram is broad and sensitivity is reduced. There were disadvantages such as the amount of sample used 1.21 times was small and the data obtained was not uniform for the entire sample.
本発明の目的は前記課題を解決した気化１３）定法及び
気化測定前処理装置を提供することにある。An object of the present invention is to provide a vaporization 13) standard method and a vaporization measurement preprocessing device that solve the above-mentioned problems.
〔発明の従来技術に対する相違点］
上述した従来の土壌、活性炭等の固体試料中の有機溶剤
成分を測定する方法に対し、本発明は、多量の試料につ
いて、測定目的成分を迅速に、安全に分離し、さらに高
感度で測定が可能となるという相違点を有する。[Differences between the invention and the prior art] In contrast to the above-mentioned conventional method for measuring organic solvent components in solid samples such as soil and activated carbon, the present invention quickly and safely measures the components to be measured in a large amount of samples. The difference is that it enables separation and measurement with even higher sensitivity.
〔課題を解決するための手段］
前記目的を達成するため、本発明に係る有機溶剤の気化
測定法においては、一定量の固体試料を加熱容器にとり
、前記固体試料中に含まれた有機溶剤成分を加熱気化す
ると共に、前記気化した有機溶剤の蒸気を真空びん中に
送気し、さらに前記真空びん中に清浄な不活性ガスを送
気して大気圧とした後、前記真空びんより測定ガスを抽
出し、該測定ガス中に含有した有機溶剤成分量を分析測
定するものである。[Means for Solving the Problems] In order to achieve the above object, in the organic solvent vaporization measurement method according to the present invention, a certain amount of a solid sample is placed in a heating container, and the organic solvent components contained in the solid sample are measured. At the same time, the vapor of the vaporized organic solvent is fed into a vacuum bottle, and a clean inert gas is fed into the vacuum bottle to bring it to atmospheric pressure. is extracted, and the amount of organic solvent contained in the sample gas is analyzed and measured.
また、本発明に係る気化測定前処理装置においては、固
体試料中に含まれる有機溶剤成分を加熱気化させる加熱
容器と、真空ポンプにより真空排気され、前記加熱容器
より気化した有機溶剤の蒸気が送気される真空びんと、
前記加熱容器内に通して清浄な不活性ガスを前記真空び
ん内に送気するテドラ−バッグとを有し、
前記加熱容器と真空びん間の配管系及び前記加熱容器と
テドラ−バッグ間の配管系のそれぞれ接合部に摺合せ面
を設け、該摺合せ面を介して前記接合部を密着させて相
互間をそれぞれ気密に接続したものである。In addition, the vaporization measurement pretreatment device according to the present invention includes a heating container that heats and vaporizes an organic solvent component contained in a solid sample, and is evacuated by a vacuum pump, and the vapor of the vaporized organic solvent is sent from the heating container. Vacuum bottles and
a Tedlar bag for supplying clean inert gas into the vacuum bottle through the heating container; a piping system between the heating container and the vacuum bottle and a piping system between the heating container and the Tedlar bag; A sliding surface is provided at each joint of the system, and the joints are brought into close contact via the sliding surface to connect each other airtightly.
［実施例］ 以下、本発明について図面を参照して説明する。[Example] Hereinafter, the present invention will be explained with reference to the drawings.
（実施例１） 第１図は本発明の実施例１を示す構成図である。(Example 1) FIG. 1 is a configuration diagram showing a first embodiment of the present invention.
図において、本発明は、固体試料中に含まれる有機溶剤
成分を加熱気化させる加熱容器１と、真空ポンプ６によ
り真空排気され、加熱容器１より気化した有機溶剤の蒸
気が送気される真空びん３と、加熱容器１内に通して清
浄な不活性ガスを真空びん３内に送気するテドラ−バッ
グ８とを有し、加熱容器１と真空びん３間の配管系及び
加熱容器１及びテドラ−バッグ８間の配管系のそれぞれ
の接合部を気密に接続したものである。該書記管系の接
合部の具体的構造について説明する。すなわち、硬質ガ
ラスなどからなる加熱容器１の開口部ｌａと接手管２を
摺合わせ面１ｂで密接させる。接手管２の他端の接手部
２ａの先端は、真空びん３の一部に設けた接手管３ａと
摺合わせ面３ｂで密接させる。In the figure, the present invention includes a heating container 1 that heats and vaporizes an organic solvent component contained in a solid sample, and a vacuum bottle that is evacuated by a vacuum pump 6 and into which vaporized organic solvent vapor is sent from the heating container 1. 3, and a Tedlar bag 8 that passes clean inert gas into the vacuum bottle 3 through the heating container 1, and includes a piping system between the heating container 1 and the vacuum bottle 3, the heating container 1, and the Tedlar bag 8. - Each joint of the piping system between the bags 8 is connected airtightly. The specific structure of the joint of the writing tube system will be explained. That is, the opening la of the heating container 1 made of hard glass or the like and the joint tube 2 are brought into close contact with each other at the sliding surface 1b. The tip of the joint part 2a at the other end of the joint tube 2 is brought into close contact with a joint tube 3a provided on a part of the vacuum bottle 3 through a sliding surface 3b.
さらに接手管２の一部に設けた開口部２ｂよりガラス管
１６を加熱容器１の底部ｌｃ付近まで挿入し、かつ、開
口部２ｂで接手管２と封着する。またガラス管１６の加
熱容器１の外側に突出した一方の先端部１６ａに摺合わ
せ面を設け、この摺合わせ面を接手管４の先端に設けた
摺合わせ面４ｂと密接させる。Furthermore, the glass tube 16 is inserted into the vicinity of the bottom lc of the heating container 1 through an opening 2b provided in a part of the joint tube 2, and is sealed to the joint tube 2 through the opening 2b. Further, a sliding surface is provided on one end portion 16a of the glass tube 16 that protrudes to the outside of the heating container 1, and this sliding surface is brought into close contact with a sliding surface 4b provided at the end of the joint tube 4.
接手管４の途中に、開閉用のコック４ａを設ける。A cock 4a for opening and closing is provided in the middle of the joint pipe 4.
真空びん３の接手管３ａ及び３ｂの途中に開閉可能なテ
フロン、ガラス等有機溶剤の吸着、吸収が少ない材質か
らなるコック３ｃ、 ３ｄを設ける。さらに真空びん３
の一部に測定用気体試料を抜き取るための開口部３ｅを
設け、シリコンゴムなどからなる栓３ｆで密封する。In the middle of the joint pipes 3a and 3b of the vacuum bottle 3, cocks 3c and 3d are provided which can be opened and closed and are made of a material such as Teflon or glass that has little adsorption or absorption of organic solvents. Furthermore, vacuum bottle 3
An opening 3e for extracting the gas sample for measurement is provided in a part of the opening 3e, and the opening 3e is sealed with a stopper 3f made of silicone rubber or the like.
次に、本発明に係る固体試料中の有機溶剤の気化測定法
について説明する。Next, a method for measuring vaporization of an organic solvent in a solid sample according to the present invention will be explained.
先ず、第１図に示すように、加熱容器１内に土壌、汚泥
、活性炭等の試料５を入れ、速やかに接手管２、さらに
コック３ｃ、 ４ａをそれぞれ閉じた真空びん３及び接
手管４を接続する。次に、真空びん３の一方の接手管３
ｂに接続している真空ポンプ６を作動させ、コック３ｄ
を開にして真空びん３を真空にした後、コック３ｄを閉
にする。次に、真空びん３のコック３Ｃを開にして、加
熱容器１内の空気の一部を真空びん３内に取り込み、加
熱容器１内を陰圧とした後、加熱器７で試料５を、測定
しようとする有機溶剤成分の沸点以上に一定時間加熱を
続け、十分に有機溶剤成分′を気化する。気化が十分性
われた時点で、次にコック４ａを徐々に開にして、接手
管４に接続したテドラーバ・ソゲ８内の高純度のヘリウ
ムカスまたは窒素カス等の不活性ガス９を送気し続け、
真空びん３内に気化した有機溶剤成分（測定ガス）１０
を送り込み、加熱容器１、真空びん３内が大気圧となっ
た時点で速やかにコック３ｃを閉にするっ
以上の操作により、固体試料中の有機溶剤成分は気体で
真空びん３中に取り込まれるため、その後、栓３ｆより
ガスタイトシリンジ１１で一定量を分取し、ガスクロマ
トグラフ等に注入して測定を行い、始めの固体試料中の
有機溶剤の濃度を求める。First, as shown in FIG. 1, a sample 5 of soil, sludge, activated carbon, etc. is placed in a heating container 1, and the joint pipe 2, and the vacuum bottle 3 and joint pipe 4 with the cocks 3c and 4a closed, respectively, are placed. Connecting. Next, one joint pipe 3 of the vacuum bottle 3
Activate the vacuum pump 6 connected to b, and turn on the cock 3d.
After the vacuum bottle 3 is evacuated by opening, the cock 3d is closed. Next, the cock 3C of the vacuum bottle 3 is opened to take some of the air inside the heating container 1 into the vacuum bottle 3, and after making the inside of the heating container 1 a negative pressure, the sample 5 is heated using the heater 7. Heating is continued for a certain period of time above the boiling point of the organic solvent component to be measured to sufficiently vaporize the organic solvent component. When sufficient vaporization is achieved, the cock 4a is gradually opened to supply an inert gas 9 such as high-purity helium scum or nitrogen scum in the Tedlar bar soge 8 connected to the joint pipe 4. continue,
Organic solvent component (measurement gas) vaporized in vacuum bottle 3 10
The organic solvent component in the solid sample is taken into the vacuum bottle 3 in the form of a gas by the above-described operation of feeding the sample and immediately closing the cock 3c when the inside of the heating container 1 and vacuum bottle 3 reach atmospheric pressure. Therefore, after that, a certain amount is collected from the stopper 3f using the gas-tight syringe 11, and the sample is injected into a gas chromatograph or the like for measurement to determine the concentration of the organic solvent in the initial solid sample.
（実施例２）
第２図は加熱容器ｌ内の試料５を加熱する方法として測
定目的の有機溶剤が加熱容器ｌ及び接手管２，３ａなど
の内壁に吸着あるいは捕集され易い比較的高い沸点のも
のに対する場合に用いる加熱例を示す。(Example 2) Figure 2 shows a method of heating a sample 5 in a heating container 1 at a relatively high boiling point at which the organic solvent to be measured is easily adsorbed or collected on the inner walls of the heating container 1 and the joint pipes 2, 3a, etc. An example of heating used for this is shown below.
図に示すように、ガスタイトシリンジ１１で加熱容器１
の周囲を加熱すれば、真空びん３に測定成分を捕集する
ための捕集効率をより高めることができる。As shown in the figure, the heating container 1 is heated with the gas tight syringe 11.
By heating the surrounding area, the collection efficiency for collecting the measurement component in the vacuum bottle 3 can be further increased.
また、１２は分取コックで、ます、分取コック１２によ
り吸引器１３及び分取管１４をシリースにつなぎ、吸引
器１３を１３ａ方向に吸引して分取管１４内を試料ガス
で十分に置換する。次に分取コック１２を切替えてガス
クロマトグラフ１５の注入系にセットして、分取管１４
内の試料ガスをガスクロマトグラフ１５に送入して測定
する。さらに、分取コック１２．吸弓器１３及びガスク
ロマトグラフ１５を連動させ、測定を自動化させること
も可能である。なお、微量測定成分を精度良く測定する
ために、真空びん３゜分取コツ９１２１分取管１４を測
定する萌にあらかじめ十分クリーンにするためにこれら
全系統を加熱しながら、不純物成分を十分除去するよう
にできることはもちろんである。In addition, 12 is a preparative cock, which connects the aspirator 13 and the preparative tube 14 to the series, and suctions the aspirator 13 in the direction 13a to fill the preparative tube 14 with sufficient sample gas. Replace. Next, switch the preparative cock 12 and set it in the injection system of the gas chromatograph 15, and
The sample gas inside is sent to the gas chromatograph 15 and measured. Furthermore, the preparative cock 12. It is also possible to automate the measurement by linking the bow absorber 13 and the gas chromatograph 15. In addition, in order to accurately measure trace amounts of components to be measured, all impurity components are thoroughly removed while heating the entire system to make the vacuum bottle 3° preparative collection tip 9121 preparative tube 14 sufficiently clean before measurement. Of course, you can do what you want.
表１に本発明の方法と従来の方法との溶媒抽出結果を示
す。Table 1 shows the solvent extraction results of the method of the present invention and the conventional method.
（以下余白）
表 １
表１の結果から明らかなように、本発明の方法によれば
、従来の溶媒抽出法に較べて高感度に測定できることが
分かる。(The following is a blank space) Table 1 As is clear from the results in Table 1, it can be seen that the method of the present invention allows measurement with higher sensitivity than the conventional solvent extraction method.
以上説明したように本発明の測定方法を用いることによ
り、
■溶媒抽出法で測定成分を抽出するには、長時間を要し
、それでも十分な抽出効率が得にくかったのに対し、本
性は、測定成分の沸点以上に加熱するため迅速に、しか
も十分な捕集率を得ることができること。As explained above, by using the measurement method of the present invention, ①It took a long time to extract the component to be measured using the solvent extraction method, and even then it was difficult to obtain sufficient extraction efficiency. Because the component is heated above the boiling point of the component to be measured, a sufficient collection rate can be obtained quickly.
■溶媒抽出法では高沸点成分も同時に抽出され、これも
同時に測定装置に注入するため、測定系を汚染してしま
うが、本性では、高沸点成分は気化しにくく、そのため
、測定系の汚染を防ぐことができること。■In the solvent extraction method, high boiling point components are also extracted at the same time and are injected into the measuring device at the same time, which can contaminate the measurement system. However, in nature, high boiling point components are difficult to vaporize, so they do not contaminate the measurement system. What can be prevented.
■試料中に水分が含まれていても、気化分離には何ら支
障をきたさないこと、
■引火性で人体に有害な薬品は全く使用しないこと、
■また従来の加熱気化法に較べ多量の試料を用いること
ができるため、得られたデータに偏りが少ないこと、
■十分に気化したものを、中゛間容器にとり、これを測
定系に入れるため、従来のように分離不十分でブロード
なりロマト測定とはならず、シャープで高精度なグロマ
トグラムのピークが得られること。しかも従来の溶媒抽
出法に較べ、より以上に高感度で測定できることなどの
効果がある。■Even if the sample contains moisture, it does not interfere with vaporization separation; ■No flammable chemicals that are harmful to the human body are used; ■Also, a large amount of sample is required compared to the conventional heating vaporization method. 1) The sufficiently vaporized material is taken into an intermediate container and put into the measurement system, which eliminates the problem of insufficient separation and broad chromatography, unlike conventional methods. It is not a measurement, but a sharp and highly accurate chromatogram peak can be obtained. Furthermore, compared to conventional solvent extraction methods, this method has the advantage of being able to perform measurements with higher sensitivity.
第１図は本発明の実施例１に係る測定方法を実施する測
定前処理装置を示す構成図、第２図は本発明の実施例２
に係る測定前処理装置を示す構成図である。
１・・・加熱容器 １ａ・・・加熱容器の開
口部ｌｂ、４ｂ・・・摺合わせ面 ＩＣ・・・加熱
容器の底部２．４・・・接手管 ２ａ・・・
接手管の接手部２ｂ・・・接手管２の開口部 ３・・
・真空びん３ａ、３ｂ・・・真空びんの接手管
３ｃ、３ｄ・・・真空び、んのコック４ａ・・・コック
５・・・試料 ６・・・真空ポンプ７・
・・加熱器 ８・・・テドラ−バッグ９・
・・不活性ガス ＩＯ・・・測定ガス１１・・
・ガスタイトシリンジ １２・・・分取コック１３・・
・吸引器 １４・・・分取管１５・・ガス
クロマトグラフFIG. 1 is a configuration diagram showing a measurement preprocessing device for carrying out a measurement method according to Example 1 of the present invention, and FIG. 2 is a configuration diagram showing Example 2 of the present invention.
FIG. 2 is a configuration diagram showing a measurement preprocessing device according to the present invention. 1...Heating container 1a...Opening part lb of heating container, 4b...Sliding surface IC...Bottom part of heating container 2.4...Joint pipe 2a...
Joint part 2b of the joint pipe... Opening part of the joint pipe 2 3...
・Vacuum bottle 3a, 3b...Vacuum bottle joint tube 3c, 3d...Vacuum bottle cock 4a...Cook 5...Sample 6...Vacuum pump 7・
・・Heater 8・Tedlar bag 9・
...Inert gas IO...Measurement gas 11...
・Gas tight syringe 12... Preparative cock 13...
・Suction device 14...Preparation tube 15...Gas chromatograph
Claims (2)
料中に含まれた有機溶剤成分を加熱気化すると共に、前
記気化した有機溶剤の蒸気を真空びん中に送気し、さら
に前記真空びん中に清浄な不活性ガスを送気して大気圧
とした後、前記真空びんより測定ガスを抽出し、該測定
ガス中に含有した有機溶剤成分量を分析測定することを
特徴とする有機溶剤の気化測定法。(1) A certain amount of solid sample is placed in a heating container, the organic solvent component contained in the solid sample is heated and vaporized, and the vapor of the vaporized organic solvent is sent into a vacuum bottle. An organic solvent characterized in that after supplying clean inert gas into the vacuum bottle to bring it to atmospheric pressure, the measurement gas is extracted from the vacuum bottle, and the amount of organic solvent components contained in the measurement gas is analyzed and measured. Vaporization measurement method.
せる加熱容器と、真空ポンプにより真空排気され、前記
加熱容器より気化した有機溶剤の蒸気が送気される真空
びんと、前記加熱容器内に通して清浄な不活性ガスを前
記真空びん内に送気するテドラ−バッグとを有し、 前記加熱容器と真空びん間の配管系及び前記加熱容器と
テドラ−バッグ間の配管系のそれぞれ接合部に摺合せ面
を設け、該摺合せ面を介して前記接合部を密着させて相
互間をそれぞれ気密に接続したことを特徴とする有機溶
剤の気化測定前処理装置。(2) A heating container that heats and vaporizes an organic solvent component contained in a solid sample, a vacuum bottle that is evacuated by a vacuum pump, and into which vaporized organic solvent vapor is sent from the heating container, and the inside of the heating container. a Tedlar bag that sends clean inert gas into the vacuum bottle through a Tedlar bag, and a piping system between the heating container and the vacuum bottle and a piping system between the heating container and the Tedlar bag are respectively connected. 1. A pretreatment device for measuring the vaporization of an organic solvent, characterized in that a sliding surface is provided at the sliding surface, and the joint portions are brought into close contact with each other via the sliding surface, thereby airtightly connecting each other.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33759289A JPH03197834A (en) | 1989-12-26 | 1989-12-26 | Method for measuring evaporation of organic solvent and pretreating device for measurement of evaporation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33759289A JPH03197834A (en) | 1989-12-26 | 1989-12-26 | Method for measuring evaporation of organic solvent and pretreating device for measurement of evaporation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03197834A true JPH03197834A (en) | 1991-08-29 |
Family
ID=18310100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33759289A Pending JPH03197834A (en) | 1989-12-26 | 1989-12-26 | Method for measuring evaporation of organic solvent and pretreating device for measurement of evaporation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03197834A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0666693A (en) * | 1992-08-20 | 1994-03-11 | Kanagawa Pref Gov | Desorption of organic chlorine based solvent and sampling tube therefor |
| JP2003035635A (en) * | 2001-07-19 | 2003-02-07 | Fujitsu Ltd | Pipe and apparatus for preparing gas |
| KR100622871B1 (en) * | 2005-07-11 | 2006-09-12 | 강원대학교산학협력단 | Emission test cell for emitting pollutants |
| CN105242008A (en) * | 2015-09-23 | 2016-01-13 | 同济大学 | Toxicant exposure testing apparatus used for regulating and controlling volatile organic compound gaseous-state pollution concentration |
| CN113908591A (en) * | 2020-07-07 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
-
1989
- 1989-12-26 JP JP33759289A patent/JPH03197834A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0666693A (en) * | 1992-08-20 | 1994-03-11 | Kanagawa Pref Gov | Desorption of organic chlorine based solvent and sampling tube therefor |
| JP2003035635A (en) * | 2001-07-19 | 2003-02-07 | Fujitsu Ltd | Pipe and apparatus for preparing gas |
| KR100622871B1 (en) * | 2005-07-11 | 2006-09-12 | 강원대학교산학협력단 | Emission test cell for emitting pollutants |
| CN105242008A (en) * | 2015-09-23 | 2016-01-13 | 同济大学 | Toxicant exposure testing apparatus used for regulating and controlling volatile organic compound gaseous-state pollution concentration |
| CN105242008B (en) * | 2015-09-23 | 2017-07-11 | 同济大学 | It is a kind of to be used to regulate and control the contamination experimental apparatus of volatile organic matter gaseous contamination concentration |
| CN113908591A (en) * | 2020-07-07 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
| CN113908591B (en) * | 2020-07-07 | 2023-03-17 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
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