JPH01165956A - Measuring method of very small quantity of water and apparatus therefor - Google Patents
Measuring method of very small quantity of water and apparatus thereforInfo
- Publication number
- JPH01165956A JPH01165956A JP62326090A JP32609087A JPH01165956A JP H01165956 A JPH01165956 A JP H01165956A JP 62326090 A JP62326090 A JP 62326090A JP 32609087 A JP32609087 A JP 32609087A JP H01165956 A JPH01165956 A JP H01165956A
- Authority
- JP
- Japan
- Prior art keywords
- acetylene
- water
- flame ionization
- ionization detector
- carbide powder
- 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 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 10
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 4
- 230000005494 condensation Effects 0.000 claims abstract description 4
- 239000012530 fluid Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 229910014813 CaC2 Inorganic materials 0.000 abstract 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract 1
- 235000011116 calcium hydroxide Nutrition 0.000 abstract 1
- 239000000920 calcium hydroxide Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（技術分野）
本発明は、気体に含まれている微量な水分を検出する技
術に関する。DETAILED DESCRIPTION OF THE INVENTION (Technical Field) The present invention relates to a technique for detecting trace amounts of moisture contained in gas.
（従来技術）
例えば、ガスクロマトグラフィによる成分の分析におい
では、過密、カラムから分Ｍされた成分を水素炎イオン
化検出器を用いて検出することが行なわれでいるが、水
分は非燃焼性であるため、イオン化せず検出が不可能で
ある。(Prior art) For example, in component analysis using gas chromatography, components separated from an overcrowded column are detected using a flame ionization detector, but water is non-flammable. Therefore, it does not ionize and cannot be detected.
このため、水分の検出か必要である場合には、水素炎イ
オン化検出器に代えで熱伝導度検出器が使用されている
が、キャリアガスとの熱伝導差により検出する関係上、
感度か低く、敢て検出感度を向上させべくプリアンプを
接続したとしてもせいぜいいｌｐｐｍ程度で、しかもＳ
／Ｎ比か低く信頼性に欠けるという問題かある。For this reason, when it is necessary to detect moisture, a thermal conductivity detector is used instead of a hydrogen flame ionization detector.
The sensitivity is low, and even if you connect a preamplifier to improve the detection sensitivity, it will only be at most lppm, and the S
The problem is that the /N ratio is low and reliability is lacking.
（目的）
本発明はこのような問題に鑑みてなされたものであって
、その目的とするところは微量な水分を高い精度と信頼
性でもって検出することかできる測定方法を提案するこ
とにある。(Purpose) The present invention was made in view of these problems, and its purpose is to propose a measurement method that can detect trace amounts of moisture with high accuracy and reliability. .
また、本発明の他の目的は、上述の方法を実施するため
の装置を提供することにある。Another object of the invention is to provide an apparatus for carrying out the above method.
（発明の概要）
すなわち、本発明か特徴とするところは、被測定流体を
カーバイト粉末に接触させて可燃性ガスであるアセチレ
ンに変換し、このアセチレンを水素炎イオン化検出器に
より検出するよう（こした点にある。(Summary of the Invention) That is, the present invention is characterized in that the fluid to be measured is brought into contact with carbide powder to be converted into acetylene, which is a flammable gas, and this acetylene is detected by a hydrogen flame ionization detector ( It's in the middle of the day.
（実施例）
そこで以下に本発明の詳細を図示した実施例に基づいて
説明する。(Example) The details of the present invention will be described below based on illustrated examples.
第１図は本発明の一実施例を示したものであって、図中
符号１は、本発明を適用するに最適なガスクロマトグラ
フ装置で、特に水分を選択的に吸着、分離するのに適し
たポーラスポリマービーズを充填剤とする分析用カラム
２を何し、流入側が試料注入口３を介してキャリアガス
源４に、排出側が後述する水分検出装置５に接続されて
いる。FIG. 1 shows one embodiment of the present invention, and the reference numeral 1 in the figure is a gas chromatograph apparatus most suitable for applying the present invention, and is particularly suitable for selectively adsorbing and separating water. The analytical column 2, which uses porous polymer beads as a filler, is connected at its inlet side to a carrier gas source 4 via a sample injection port 3, and at its outlet side to a moisture detection device 5, which will be described later.
５は、本発明か特徴とする前述の水分装置で、図中符号
６は、ヒータ７により結露温度以上に加熱された容器に
カーバイト（ＣａＣｚ）の粉末９を充填してなる反応管
で、−側が分析用カラム２の排出口に、他側か水素炎イ
オン化検出器１０に接続されでいる。5 is the above-mentioned moisture device which is a feature of the present invention, and the reference numeral 6 in the figure is a reaction tube formed by filling a container with carbide (CaCz) powder 9, which is heated by a heater 7 to a temperature higher than the dew condensation temperature. The - side is connected to the outlet of the analytical column 2, and the other side is connected to the hydrogen flame ionization detector 10.
この実施例において、試料注入口３からサンプルを注入
すると、サンプル中の水分は、分析用カラム２により定
まるリテンションタイムでもってキャリアガスとともに
反応管６に排出される。In this embodiment, when a sample is injected from the sample injection port 3, water in the sample is discharged into the reaction tube 6 together with the carrier gas at a retention time determined by the analytical column 2.
キャリアガスとともに排出された水分は、反応管６内で
結露を生しることなくカーバイト粉末９に接触して
ＣａＣｚ＋２Ｈ２０→
Ｃ２Ｈ２＋Ｃａ （○Ｈ）２
なる反応によりアセチレンに変換される。このアセチレ
ンは、水素炎イオン化検出器１０に流入し、その可燃性
の故に水素炎イオン化検出器か備える高い感度でもって
検出されることになる。The moisture discharged together with the carrier gas comes into contact with the carbide powder 9 in the reaction tube 6 without condensation, and is converted into acetylene by the reaction CaCz+2H20→C2H2+Ca (○H)2. This acetylene flows into the flame ionization detector 10 and, because of its flammability, will be detected with the high sensitivity that a flame ionization detector has.
なあ、この実施例においては、ガスクロマトグラフ用検
出器として用いる場合を例に採って説明したか、微量な
水分の含有か問題となる気体、例えば標準ガス等に含ま
れている微量な水分の測定に適用できることは明らかで
ある。By the way, in this example, we have explained the case where it is used as a detector for gas chromatography, or it is used to measure a trace amount of water contained in a gas that may contain a trace amount of water, such as a standard gas. It is clear that it can be applied to
［実 施 例］
乾燥窒素ガスに１０ｐｌ）ｍの水分を含有させたサンプ
ル％１ｍｆｌ注入して、３回の測定したところ、第２図
（Ｉ）乃至（ＩＩＩ）に示したように、高い再現性でも
って測定することかできた。[Example] When 1 mfl of a sample containing 10 pl) m of moisture in dry nitrogen gas was injected and measurements were performed three times, high reproducibility was obtained as shown in Figures 2 (I) to (III). It was possible to measure it by gender.
また検出限界を確認するため、水分量を変化させながら
測定したところ、プリアンプを必要とすることなく０．
ｌｐｐｍまで検出することかでき、熱伝導度検出器を使
用した場合に比較しで高いＳ／Ｎ比でもって従来の１／
１０程度の低濃度の水分を検出できることが解った。In addition, in order to confirm the detection limit, we measured while changing the moisture content and found that the detection limit was 0.
It can detect down to lppm, and has a higher S/N ratio than when using a thermal conductivity detector, which is 1/1 of the conventional one.
It was found that water at concentrations as low as 10% can be detected.
（効果）
以上、説明したように本発明によれば、被測定流体をカ
ーバイト粉末に接触させてアセチレンに変換し、このア
セチレンを水素炎イオン化検出器により検出するように
したので、水素炎イオン化検出器か固有的に備えている
高い感度でもって水分を検出することができる。(Effects) As explained above, according to the present invention, the fluid to be measured is brought into contact with carbide powder to be converted into acetylene, and this acetylene is detected by a flame ionization detector. Moisture can be detected with the inherent high sensitivity of the detector.
第１図は本発明の一実施例をガスクロマトグラフ装置に
適用したものの構成図、及び第２図（Ｉ）乃至（１）は
、それぞれ同上装置による測定結果の一例を示す線図で
ある。
１・・・・分析用力う八 ６・・・・反応管７・・・
・ヒータ ９・・・・カーバイト粉末１０・・
・・水素炎イオン化検出器FIG. 1 is a block diagram of an embodiment of the present invention applied to a gas chromatograph device, and FIGS. 2(I) to (1) are diagrams showing examples of measurement results by the same device. 1... Analytical power 8 6... Reaction tube 7...
・Heater 9...Carbide powder 10...
・Hydrogen flame ionization detector
Claims (2)
レンに変換する工程と、前記アセチレンを水素炎イオン
化検出器により検出する工程からなる微量水分の測定方
法。(1) A method for measuring trace amounts of moisture, which comprises the steps of bringing the fluid to be measured into contact with carbide powder to convert it into acetylene, and detecting the acetylene with a flame ionization detector.
化検出器に連通する容器に、カーバイト粉末を充填する
とともに、前記容器を結露温度以上に加熱してなる微量
水分測定装置。(2) A trace moisture measuring device in which carbide powder is filled in a container whose one side communicates with a gas inlet to be measured and the other side communicates with a hydrogen flame ionization detector, and where the container is heated to a temperature above dew condensation temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62326090A JPH01165956A (en) | 1987-12-22 | 1987-12-22 | Measuring method of very small quantity of water and apparatus therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62326090A JPH01165956A (en) | 1987-12-22 | 1987-12-22 | Measuring method of very small quantity of water and apparatus therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01165956A true JPH01165956A (en) | 1989-06-29 |
Family
ID=18183992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62326090A Pending JPH01165956A (en) | 1987-12-22 | 1987-12-22 | Measuring method of very small quantity of water and apparatus therefor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01165956A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015108600A (en) * | 2013-12-05 | 2015-06-11 | 株式会社堀場エステック | Gas chromatograph, and gas chromatograph intermediate processing apparatus |
-
1987
- 1987-12-22 JP JP62326090A patent/JPH01165956A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015108600A (en) * | 2013-12-05 | 2015-06-11 | 株式会社堀場エステック | Gas chromatograph, and gas chromatograph intermediate processing apparatus |
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