JPH0333654A - Process gas chromatograph - Google Patents
Process gas chromatographInfo
- Publication number
- JPH0333654A JPH0333654A JP16833989A JP16833989A JPH0333654A JP H0333654 A JPH0333654 A JP H0333654A JP 16833989 A JP16833989 A JP 16833989A JP 16833989 A JP16833989 A JP 16833989A JP H0333654 A JPH0333654 A JP H0333654A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- detector
- liquid
- column
- evaporator
- 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
- 238000000034 method Methods 0.000 title claims description 11
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims description 23
- 239000006200 vaporizer Substances 0.000 claims description 13
- 238000013375 chromatographic separation Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発１１は、キャピラリカラムを用いて試料中の被測定
成分を連続分析するのに好適なプロセスガスクロマトグ
ラフに関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a process gas chromatograph suitable for continuous analysis of a component to be measured in a sample using a capillary column.
〈従来の技術〉
１９５２年にＡ、Ｊ、Ｐ、Ｍａｒｔｉｎによって発表さ
れたカスクロマトグラフィは、揮発性化合物の画期的な
分析方法であり、以来今日まで種々の改良が加えられ分
析化学の分野で広く使用されている。このようなガスク
ロマトグラフィを利用し、石油プラント等における各種
流体に含まれる被測定成分を連続的かつ再現性良く分析
する装置としてプロセスガスクロマトグラフが開発され
、広い分野で使用されている。第２図は、このようなプ
ロセスガスクロマトグラフの要部構成説明図であり、図
中、１は第１乃至第６の内部接続「１１ａ〜１ｆと内部
計量管１ｇ（例えは内容積１μｌであり第３接続「１１
Ｃと第６接続１．１１ ｆを結ぶ部分）を有する試料採
取弁、２は第１乃至第４の接続口を有し内部流路か実線
状態と破線状態に交互に切換えられる第１切換弁、３は
第１乃至第４の接続【」３ａ〜３ｄを有し第１切換弁と
連動しながら内部流路が実線状態と破線状態に交互に切
換えられる第２切換弁、４．ａ−′−４ｃは内部にカラ
ム充填剤が充填されてなる分ｉ１ｉ＋［カラム、５ａ〜
５Ｃは流体抵抗を調整できるレストリフタ、６は第１乃
至第４の接続１」６ａ〜６ｄを有し第１切換弁と通勤し
ながら内部流路か実線状態と破線状態に交互に切換えら
れる第３切換弁、７は例えば熟伝導度検出器でなる検出
器である。また、領域Ａは例えば３００°Ｃに保たれ、
領域Ｂは例えば１２０゜Ｃに保たれてる。<Prior art> Cas chromatography, introduced by A.J.P. Martin in 1952, is a groundbreaking analytical method for volatile compounds.Since then, various improvements have been made and it has become popular in the field of analytical chemistry. Widely used. Process gas chromatographs have been developed as devices that utilize such gas chromatography to continuously and reproducibly analyze components to be measured contained in various fluids in oil plants and the like, and are used in a wide range of fields. FIG. 2 is an explanatory diagram of the main part structure of such a process gas chromatograph. Third connection “11
2 is a sampling valve having a first to fourth connection ports and is alternately switched between an internal flow path and a solid line state and a broken line state. , 3 is a second switching valve having first to fourth connections 3a to 3d and whose internal flow path is alternately switched between a solid line state and a broken line state while interlocking with the first switching valve; 4. a-'-4c is the column i1i+[column, 5a~
5C is a rest lifter that can adjust the fluid resistance; 6 is a third connection having first to fourth connections 1'' 6a to 6d; the internal flow path is alternately switched between a solid line state and a broken line state while commuting with the first switching valve; The switching valve 7 is a detector consisting of, for example, a conductivity detector. In addition, area A is maintained at 300°C, for example,
Region B is maintained at, for example, 120°C.
このような要部構成からなる従来のプロセスカスクロマ
ｌ−グラフにおいて、試料採取弁１の内部計量管１ｇに
液体試料が供給されている状態で試料採取弁１をオンに
すると、該試料採取弁の内部流路か実線状態から破線状
態に切換えられる。このため、キャリアカスが、試料採
取弁１の第１接続１」１ａ→内部計量管１ｇ→試料採取
弁１の第２接続Ｌｌ １ ｂ→第第２切換２の第４及び
第３接続口２ｄ、２ｃの流路で流ｉｔて、ｌ記液体試料
を気化しながら分離カラム４ａに搬送する。また、分離
カラム４ａの溶出カスは、第３切換え弁６の第１及び第
２接続目６ａ、６ｂ→分離カラム４ｃと搬送されてクロ
マトグラフィツクに分離され、その後、検出器７で挽出
されて被測定成分濃度信号を与えるようになる。In the conventional process gas chroma l-graph having such a main part configuration, when the sample sampling valve 1 is turned on with a liquid sample being supplied to the internal measuring tube 1g of the sample sampling valve 1, the sample sampling valve 1 turns on. The internal flow path is switched from the solid line state to the broken line state. For this reason, the carrier scum is transferred from the first connection 1'' 1a of the sample sampling valve 1 to the internal metering pipe 1g to the second connection Ll 1 b of the sample sampling valve 1 to the fourth and third connection ports 2d of the second switch 2. , 2c, the liquid sample is vaporized and transported to the separation column 4a. Further, the eluted residue from the separation column 4a is transported from the first and second connections 6a and 6b of the third switching valve 6 to the separation column 4c, separated by chromatography, and then extracted by the detector 7. A concentration signal of the component to be measured is given.
〈発明が解決しようとする問題点〉
然しなから、上記従来例においては、試料採取弁１の内
部計量管１ｇに供給される液体の圧力か５／Ｅｉ９／Ｃ
ｍ、’以上になると液体の洩れか生ずるため、液体試料
の圧力を５１９／Ｃｍ、２以下にしなければならなかっ
た。このため、低沸点の気化しやすい成分を含む液体試
料を分析できないという欠点があった。また、領域Ｂの
温度を高くし試料採取弁１の温度を高くすると、試料採
取弁１の内部計量管１ｇ付近で重合か起こるため、加熱
すると重合する成分を含む液体試料は分析できないとい
う欠点もあった。<Problem to be solved by the invention> However, in the above conventional example, the pressure of the liquid supplied to the internal measuring tube 1g of the sampling valve 1 is 5/Ei9/C.
If the pressure exceeds m,', the liquid will leak, so the pressure of the liquid sample had to be lower than 519/Cm,2. For this reason, there was a drawback that liquid samples containing easily vaporized components with low boiling points could not be analyzed. In addition, if the temperature of region B is increased and the temperature of the sample sampling valve 1 is increased, polymerization will occur near the internal measuring tube 1g of the sample sampling valve 1, so there is also the disadvantage that liquid samples containing components that polymerize when heated cannot be analyzed. there were.
本発明は、かかる従来例の欠点に鑑みてなされたもので
あり、その目的は、供給される液体試料の圧力か高くと
も液体の洩れが生ぜず、且つ、微量の液体試料をシャー
プに（即ち、切れの良い状態で）採取できる試料採取弁
を（６１Ａえたプルセス刃スクロマトグラフを提１共す
ることにある。The present invention was made in view of the drawbacks of the conventional examples, and its purpose is to prevent liquid from leaking even if the pressure of the liquid sample to be supplied is high, and to sharpen a small amount of liquid sample (i.e. The objective is to provide a 61A Purcess blade chromatograph with a sample collection valve that allows sampling (in a sharp state).
く問題点を解決するだめの手段〉
本発明は、プロセスカスクロマ１〜グラフにおいて、キ
ャリアカスか導入され液体試料を気化する気化器と、該
気化器に液体試料を供給するキャピラリ−ヂ５２．−ブ
と、内容積一定の外付計量管を有する試料採取弁と、分
離カラムを７１゛するカラムシステムと、該カラムシス
テムから溶出する成分を検出する検出器とを設け、前記
気化器、キャピラリ−チｌ−ブ、及び試料採取弁がそれ
ぞれ個別に温度調節されるように椙戒することによって
前記問題点を１４１’決したものである。Means for Solving Problems> The present invention provides a vaporizer for vaporizing a liquid sample into which a carrier cass is introduced, and a capillary 52 for supplying the liquid sample to the vaporizer in the process gas chroma 1 to graph. - a sampling valve having an external metering tube with a constant internal volume, a column system having a separation column of 71゜, and a detector for detecting components eluted from the column system; The above-mentioned problem has been resolved by making sure that the temperature of the tube and sampling valve are individually controlled.
また、本発１男は、プロセスガスクロマトグラフにおい
て、キャリアカスか導入され液体試料を気化する気化器
と、該気化器に液体試料を供給するキャピラリーチュー
ブと、内容積一定の外付計量管を有する試料採取弁と、
分離カラムを有するカラムシステムと、該カラムシステ
ムから溶出する成分を検出する検出器とを設け、前記気
化器、キャピラリーチューブ、及び試料採取弁がそれぞ
れ個別に温度調節されるように構成すると共に、試料採
取弁で採取された試料を前記分離カラムを通さずに検２
１１器に導くことと、試料採取弁で採取された試料を前
記分離カラムを通しクロマトグラフィツクに分離しての
ち検出器に導くことを交互に行なうことによって前記問
題点を解決したものである。In addition, the first inventor has a process gas chromatograph that has a vaporizer into which a carrier gas is introduced and vaporizes a liquid sample, a capillary tube that supplies the liquid sample to the vaporizer, and an external measuring tube with a constant internal volume. a sampling valve;
A column system having a separation column and a detector for detecting components eluted from the column system are provided, and the vaporizer, the capillary tube, and the sample collection valve are each configured to be individually controlled in temperature, and The sample collected with the sampling valve is detected without passing through the separation column.
This problem has been solved by alternately conducting the sample collection through the separation column, chromatographically separating the sample through the separation column, and then introducing the sample to the detector.
史に、本発明は、プ１：７セスカスクロマ）・グラフに
おいて、キャリアカスが導入され液体試料を気化する気
化器と、該気化器に液体試料を供給するキャピラリーチ
ューブと、内容積一定の外付計量がら該試料を分析でき
るようになる。Historically, the present invention is based on a vaporizer that vaporizes a liquid sample into which a carrier gas is introduced, a capillary tube that supplies the liquid sample to the vaporizer, and an external capillary tube with a constant internal volume. The sample can be analyzed while weighing.
尚、本発明は上述の実施例に限定されることなく種々の
変形が可能であり、例えは試料採取弁１１の第５接続１
］ １１ ｅから排：１１される試料を検１．Ｈ器７を
経由させて廃棄するような組成にし該試料を常時監視す
るようにしても良い。また、第１図のキャピラリーカラ
ム４ｂに代えて流体抵抗値の可変が容易なレス１ヘリク
タを用いても良いものとする。Note that the present invention is not limited to the above-described embodiments, and can be modified in various ways. For example, the fifth connection 1 of the sample sampling valve 11
] 11 Discharge from e: 11 Inspect the sample 1. The composition may be such that the sample is discarded via the H vessel 7, and the sample may be constantly monitored. In addition, in place of the capillary column 4b in FIG. 1, a less helictor whose fluid resistance value can be easily varied may be used.
〈発明の効果〉
以」二詳しく説明したような本発明によれば、供給され
る液体試料の圧力が高くとも液体の洩れか生ぜず、且つ
、微量の液体試料をシャープに採取できる試料採取弁を
倫えたブルセスガスク１コマドグラフが実現する。<Effects of the Invention> According to the present invention as described in detail below, there is provided a sample sampling valve that does not cause any liquid leakage even when the pressure of the supplied liquid sample is high, and can sharply collect a small amount of liquid sample. A Bourses-Gasque one-frame graph is realized.
また、下記■〜■のような利点もある。即ち、■高温、
高圧雰囲気になる気化器に可動部かないため、長期間ノ
ーメンテナンスで動作する。■気化された試料を試料採
取弁でカスサンプリングするため、微量の試料をシャー
プにサンプリングで１
きる。従って、分離カラムとしてキャピラリーカラムを
使用するときなどに用いて奸適である。■高圧部にシー
ルを必要とする部分かないため、高圧状態の試料をもサ
ンプリングか旬能である。また、前記従来例のようなリ
ークが生ずる心配もない。■温度調節する部分が領域Ａ
〜Ｈの５部分に分割されているため、各部分（気化器、
試料採取弁、及び分１ｌｉｆｆカラムなど）をＲ適な温
度に選定できる。このため、沸点の異なる神々の試料に
対厖できる。■試料の性状（例えば粘土）か変化するこ
とによって生ずるサンプルボリウムの変化を補正するこ
とにより、試料の性状変化による誤差を回避して再現性
よく試料を分析できる。In addition, there are also advantages such as the following. Namely, ■high temperature;
There are no moving parts in the vaporizer, which creates a high-pressure atmosphere, so it can operate without maintenance for long periods of time. ■Since the vaporized sample is sampled using the sampling valve, a very small amount of sample can be sampled sharply. Therefore, it is suitable for use when a capillary column is used as a separation column. ■Since there are no high-pressure parts that require seals, it is possible to sample samples under high pressure. Further, there is no fear of leakage occurring as in the conventional example. ■The part that adjusts the temperature is area A.
Since it is divided into 5 parts of ~H, each part (vaporizer,
(sampling valve, minute liff column, etc.) can be selected to the appropriate temperature. Therefore, it can be used for samples with different boiling points. (2) By correcting changes in the sample volume caused by changes in the properties of the sample (for example, clay), it is possible to avoid errors caused by changes in the properties of the sample and analyze the sample with good reproducibility.
第１図は本発明実施例の構成説明図、第２図は従来例の
構成説明図である。
１．１１・・・・・・試料採取弁、２，３．６・・・・
・・切換弁、４ａ〜４Ｃ・・・・・・分離カラム、４ｄ
・・・ダミーカラム、５ａ〜５ｄ・・・・・・レス１ヘ
リクタ、７・・・・・・検出器８ａ、８ｂ・・・・・・
圧力計、９・・・・・・減圧弁、２
０・・・・・・フロ
メ
タ、
１・・・・・・試料採取弁、
２・・・・・・気化器FIG. 1 is an explanatory diagram of the configuration of an embodiment of the present invention, and FIG. 2 is an explanatory diagram of the configuration of a conventional example. 1.11... Sample collection valve, 2,3.6...
...Switching valve, 4a to 4C...Separation column, 4d
...Dummy column, 5a to 5d...Res 1 helictor, 7...Detector 8a, 8b...
Pressure gauge, 9... pressure reducing valve, 2 0... flometa, 1... sampling valve, 2... vaporizer
Claims (3)
器と、該気化器に液体試料を供給するキャピラリーチュ
ーブと、内容積一定の外付計量管を有する試料採取弁と
、分離カラムを有するカラムシステムと、該カラムシス
テムから溶出する成分を検出する検出器とを具備し、前
記気化器、キャピラリーチューブ、及び試料採取弁がそ
れぞれ個別に温度調節されることを特徴とするプロセス
ガスクロマトグラフ。(1) A vaporizer into which a carrier gas is introduced to vaporize a liquid sample, a capillary tube that supplies the liquid sample to the vaporizer, a sample collection valve with an external measuring tube with a constant internal volume, and a column with a separation column. A process gas chromatograph comprising a system and a detector for detecting components eluted from the column system, wherein the vaporizer, capillary tube, and sampling valve are each individually temperature-controlled.
において、試料採取弁で採取された試料を前記分離カラ
ムを通さずに検出器に導くことと、試料採取弁で採取さ
れた試料を前記分離カラムを通しクロマトグラフイック
に分離してのち検出器に導くことを交互に行なうことを
特徴とするプロセスガスクロマトグラフ。(2) In the process gas chromatograph according to claim (1), the sample collected by the sampling valve is guided to the detector without passing through the separation column, and the sample collected by the sampling valve is guided to the separation column. A process gas chromatograph is characterized in that it alternately performs chromatographic separation through gas and then guiding the gas to a detector.
において、試料採取弁を経由した試料を前記カラムシス
テムを通すことなく検出器に導くことを特徴とするプロ
セスガスクロマトグラフ。(3) The process gas chromatograph according to claim (1), wherein the sample that has passed through the sample sampling valve is guided to the detector without passing through the column system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16833989A JPH0333654A (en) | 1989-06-30 | 1989-06-30 | Process gas chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16833989A JPH0333654A (en) | 1989-06-30 | 1989-06-30 | Process gas chromatograph |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0333654A true JPH0333654A (en) | 1991-02-13 |
Family
ID=15866227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16833989A Pending JPH0333654A (en) | 1989-06-30 | 1989-06-30 | Process gas chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0333654A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558321A (en) * | 2013-10-29 | 2014-02-05 | 徐继承 | Gas examination sample introduction evaporator with gas feeding adjusting replacing combination valve |
| JP2015200637A (en) * | 2014-03-31 | 2015-11-12 | 富士フイルム株式会社 | Recovery solvent analysis method and unit, solvent recovery preparation method, and solvent film formation method |
-
1989
- 1989-06-30 JP JP16833989A patent/JPH0333654A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558321A (en) * | 2013-10-29 | 2014-02-05 | 徐继承 | Gas examination sample introduction evaporator with gas feeding adjusting replacing combination valve |
| CN103558321B (en) * | 2013-10-29 | 2014-11-26 | 徐继承 | Gas examination sample introduction evaporator with gas feeding adjusting replacing combination valve |
| JP2015200637A (en) * | 2014-03-31 | 2015-11-12 | 富士フイルム株式会社 | Recovery solvent analysis method and unit, solvent recovery preparation method, and solvent film formation method |
| TWI651533B (en) * | 2014-03-31 | 2019-02-21 | 日商富士軟片股份有限公司 | Recovery solvent analysis method and unit, solvent recovery preparation method, and solution film formation method |
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