JPS6350751A - On-line analyzer of moisture in gaseous specimen - Google Patents
On-line analyzer of moisture in gaseous specimenInfo
- Publication number
- JPS6350751A JPS6350751A JP19396886A JP19396886A JPS6350751A JP S6350751 A JPS6350751 A JP S6350751A JP 19396886 A JP19396886 A JP 19396886A JP 19396886 A JP19396886 A JP 19396886A JP S6350751 A JPS6350751 A JP S6350751A
- Authority
- JP
- Japan
- Prior art keywords
- specimen
- moisture
- reagent
- gaseous
- gas
- 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.)
- Granted
Links
- 238000004448 titration Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 230000003287 optical effect Effects 0.000 claims abstract description 6
- 239000003021 water soluble solvent Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 18
- 239000002904 solvent Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 54
- 239000000523 sample Substances 0.000 description 37
- 238000004458 analytical method Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、気体試料中の水分をオンラインで高精度の分
析を行う装置に関するものであり、特にカールフィッシ
ャー試薬を用いた水分分析装置に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an apparatus for analyzing moisture in a gas sample with high precision online, and particularly to a moisture analyzer using a Karl Fischer reagent.
（従来の技術）
気体試料中の水分のオンライン分析する方法は、ガスク
ロマトグラフによる方法や気体試料を冷却して水分を凝
縮させて測定する凝縮法などがある。(Prior Art) Methods for online analysis of moisture in a gas sample include a gas chromatograph method and a condensation method in which the gas sample is cooled to condense moisture and then measured.
カールフィッシャー法は、液体試料の分析に用いられる
方法であり、カールフィッシャー試薬（ＫＦ試薬と称す
る。）による滴定で微量の水分が正確に測定でき、ＪＩ
Ｓ、日本薬局法、ＡＳＴＭ、ＤＩＮ等で法的な水分測定
法として採用されている。The Karl Fischer method is a method used to analyze liquid samples, and allows for accurate measurement of minute amounts of water by titration with Karl Fischer reagent (referred to as KF reagent).
It is adopted as a legal moisture measurement method by S, Japanese Pharmacopoeia Law, ASTM, DIN, etc.
カールフィッシャー分析計では、一定の試料を滴定瓶に
採取し１、これをＫＦ試薬で滴定し１滴定終点を電気的
に検出する。即ちこの分析計は、試料液に浸した双極白
金電極間に微小の電流を流しておき、試料液をＫＦ試薬
で滴定すると、試料中に水分がある間は、ＫＦ試薬と水
の反応によりヨウ化物を生じ分極して電流が流れないが
、水分が無くなるに従ってヨウ素が遊離し、急に電流が
流れるので、この電流の変化を検知して終点を求める方
法によるものであり、液体試料用の水分分析計として、
実験室用の自動分析計が販売されている。In the Karl Fischer analyzer, a certain sample is taken into a titration bottle, titrated with a KF reagent, and the titration end point is detected electrically. In other words, in this analyzer, a minute current is passed between bipolar platinum electrodes immersed in a sample solution, and when the sample solution is titrated with a KF reagent, as long as there is water in the sample, iodine is produced by the reaction between the KF reagent and the water. However, as the moisture disappears, iodine is liberated, and a current suddenly flows.This method detects changes in this current and determines the end point. As an analyzer,
Automated analyzers for laboratory use are commercially available.
（発明が解決しようとする問題点）
前述の如く、気体試料中の水分のオンライン分析には、
ガスクロマトグラフによる方法や、凝縮法が用いられる
が、その精度が低く、化学装置等で必要とされる数ｐｐ
ｍ〜数十ｐｐｍ程度の分析には不向きである。(Problems to be Solved by the Invention) As mentioned above, online analysis of moisture in a gas sample requires
Methods using gas chromatography and condensation methods are used, but their accuracy is low and only a few ppm is required for chemical equipment.
It is unsuitable for analysis of about m to several tens of ppm.
即ちガスクロマトグラフによる分析は、熱伝導度法のみ
が用いられ９分析端度は０．１％が限度である。また凝
縮法は、特殊な場合のみに用いられるが、冷熱源が必要
であり、また水辺外の凝縮物が含まれるため、精度が低
く、一般の化学装置等での分析には不向きである。That is, in the analysis by gas chromatography, only the thermal conductivity method is used, and the limit of the analytical precision is 0.1%. The condensation method is used only in special cases, but it requires a cold source and contains condensate from outside the water, so it has low accuracy and is unsuitable for analysis with general chemical equipment.
カールフィッシャー分析計は分析精度が高いが、気体試
料の場合はＫＦ試薬による滴定が直接できないため、液
体試料のみに用いられる。Although the Karl Fischer analyzer has high analytical accuracy, it is used only for liquid samples because it cannot directly titrate gas samples with the KF reagent.
（問題点を解決するための手段）
発明者は以上の如き問題点を有し、実質上不可能となっ
ている気体試料中の１ｆｆｉ水分のオンライン分析に関
し、カールフィッシャー分析計を用い、これに気体試料
採取用の装置を取り付ければ。(Means for Solving the Problems) The inventor has developed an online analysis of 1ffi water in a gas sample, which has the above-mentioned problems and is virtually impossible, using a Karl Fischer analyzer. If equipped with a device for gas sampling.
この分析を高精度で行なえることを見出し８本発明に至
った。It was discovered that this analysis could be carried out with high accuracy, leading to the present invention.
カールフィッシャー分析計で気体試料中の水分を測定す
るには、まず水溶性の溶媒を滴定量に入れ、ＫＦ試薬で
の滴定より、この溶媒を無水状態とした後、一定量の気
体試料をシールされた滴定量に吹き込み、水分を吸収さ
せる。水分吸収後の気体試料の量はガスメーターで測定
するが、その測定はガスメーターの指針が光センサーを
通過する時に得られるパルス数を数えることにより行わ
れる。水分を吸収した溶媒をＫＦ試薬で滴定し。To measure water in a gas sample with a Karl Fischer analyzer, first add a water-soluble solvent to the titration volume, make the solvent anhydrous through titration with KF reagent, and then seal a certain amount of the gas sample. Blow into the titrated amount to absorb moisture. The amount of gas sample after absorption of water is measured with a gas meter by counting the number of pulses obtained when the pointer of the gas meter passes an optical sensor. Titrate the solvent that has absorbed water with KF reagent.
その滴定量および水分吸収後のガス量を換算することに
より、気体試料中の水分が測定される。The water content in the gas sample is measured by converting the titration amount and the amount of gas after water absorption.
即ち本発明は、シールされた滴定量に水溶性の溶媒を入
れ、カールフィッシャー試薬で無水状態とした後、オン
ラインで気体試料を吹き込み水分を吸収させ、当該吸収
液中の水分をカールフィッシャー試薬で滴定すると共に
、吸収後の気体試料をガスメーターに通過させて、当該
ガスメーターの指針の回転を光センサーで読み取ること
により、気体試料量を測定し、カールフィッシャー試薬
の滴定による水分量と気体試料量からの換算によって、
気体試料中の水分濃度を測定することを特徴とする気体
試料中の水分のオンライン分析装置である。That is, in the present invention, a water-soluble solvent is put into a sealed titration volume, made anhydrous using a Karl Fischer reagent, and then a gas sample is blown on-line to absorb water, and the water in the absorption liquid is removed using a Karl Fischer reagent. At the same time as titration, the gas sample after absorption is passed through a gas meter and the rotation of the pointer of the gas meter is read with an optical sensor to measure the amount of gas sample, and the amount of gas sample is determined from the amount of water and the amount of gas sample obtained by titration of Karl Fischer reagent. By converting
This is an online analysis device for moisture in a gas sample, which is characterized by measuring the moisture concentration in the gas sample.
本分析装置は液体試料測定用のカールフィッシャー分析
装置を気体試料分析用に改造するものであり、従って液
体試料および気体試料の両者の分析ができる。また小型
電算機を組み込んで試料採取時間の指示および試料採取
ｆｆｉ、 ＫＦ試薬の滴定量および水分吸収後のガス量
よりの水分濃度の計算１分析結果の指示および外部調節
計への信号の出力などをこれにより行わせる方法がとら
れる。This analyzer is a Karl Fischer analyzer for measuring liquid samples that has been modified for gas sample analysis, and is therefore capable of analyzing both liquid and gas samples. In addition, a small computer is incorporated to instruct the sample collection time, sample collection ffi, calculate the water concentration from the titration amount of the KF reagent and the amount of gas after water absorption 1. Instruct the analysis results, and output signals to the external controller. A method is adopted in which this is done.
次に図面を用いて本発明を説明する。第一図は本発明に
よるオンライン分析装置の構成図である。Next, the present invention will be explained using the drawings. FIG. 1 is a block diagram of an online analysis device according to the present invention.
本装置は本発明による試料導入および滴定装置の部分と
、市販のカールフィッシャー水分計４．コントローラー
８（演算器付シーケンサ−）および外部調節計９に大き
く分けられる。The device consists of parts of the sample introduction and titration device according to the invention and the commercially available Karl Fischer moisture meter 4. It can be broadly divided into a controller 8 (sequencer with computing unit) and an external controller 9.
液体試料は定量ポンプ１に入り、一定量の試料が滴定量
２に送られる。滴定瓶中のスターテ−３により攪拌され
ながら、カールフィッシャー水分計中にある試薬ポンプ
５によりＫＦ試薬が注入され９滴定される。滴定瓶中に
は白金電極が装備されており、ＫＦ試薬による滴定の終
点を検知し。The liquid sample enters the metering pump 1 and a fixed amount of sample is delivered to the titration volume 2. While being stirred by the starter 3 in the titration bottle, the KF reagent is injected by the reagent pump 5 in the Karl Fischer moisture meter and titrated. The titration bottle is equipped with a platinum electrode that detects the end point of titration with the KF reagent.
増幅アンプ７を経て９滴定量点の信号がコントローラー
８へ送られる。The signal of the 9 titration point is sent to the controller 8 via the amplification amplifier 7.
気体試料中の水分の分析を行う場合には、予め水溶性溶
媒を入れて気体試料が漏れないようにシールした滴定量
に、気体試料採取用の電磁弁１０より気体試料を導入し
、その水分吸収後の気体試料量をガスメーター１３で測
定する。一定量の気体試料を導入した後、電磁弁１０を
閉止し、液体試料と同様の方法で溶媒中に含有する水分
を測定し、コントローラー４の中にある演算器により気
体試料中の水分を計算する。When analyzing moisture in a gas sample, the gas sample is introduced through the solenoid valve 10 for gas sample collection into a titration volume that has been filled with a water-soluble solvent and sealed to prevent the gas sample from leaking. The amount of gas sample after absorption is measured with a gas meter 13. After introducing a certain amount of gas sample, the solenoid valve 10 is closed, the water content in the solvent is measured in the same manner as for liquid samples, and the water content in the gas sample is calculated by the calculator in the controller 4. do.
１１は液ガス試料切換用の三方弁であり、液体試料の分
析時は三方弁を除湿器１２側に切換えて大気に解放とす
る。Reference numeral 11 denotes a three-way valve for switching liquid gas samples, and when analyzing a liquid sample, the three-way valve is switched to the dehumidifier 12 side and released to the atmosphere.
コントローラー４中には小型電算機が組み込まれ、定量
ポンプ１及び試薬ポンプ５の駆動停止。A small computer is built into the controller 4, and the metering pump 1 and reagent pump 5 are stopped.
電磁弁１０の開閉、三方弁１１の切換、スターテ−３の
駆動など必要な信号を各機器に送り制御する。Necessary signals such as opening and closing of the electromagnetic valve 10, switching of the three-way valve 11, and driving of the starter 3 are sent to and controlled by each device.
採取ガス量の測定はガスメーター１３の文字盤上に充所
プレートを取りつけ、ガスメーターの指針の動きにより
、光センサーでパルス数を読み取り、そのパルス数から
通過ガス量を求める。To measure the amount of gas to be sampled, a filling plate is attached to the dial of the gas meter 13, the number of pulses is read by an optical sensor as the pointer of the gas meter moves, and the amount of passing gas is determined from the number of pulses.
光センサーは通常赤外線式のものを用いる。文字盤上の
充所プレートの数を多くすれば、パルス数が多くなり、
精度が向上するが１通常は充所プレートを文字盤に４〜
８個設置する。The optical sensor usually uses an infrared type. If you increase the number of filled plates on the dial, the number of pulses will increase,
Accuracy improves, but 1. Normally, the full plate is placed on the dial.
Install 8 pieces.
気体試料中の水分測定のための溶媒としては。As a solvent for measuring moisture in gaseous samples.
水分を大量に溶解し、気体試料中の他の成分の溶解量が
少なく、且つ溶媒の蒸気圧の低い物質が好ましい。実際
上は溶媒の価格も考慮して、メタノール、エタノール、
ジメチルホルムアミドなどが使用される。水分測定前に
ＫＦ試薬にて溶媒を無水状態とする必要があることから
、使用する溶媒はできるだけ水分の少ないものが好まし
い。It is preferable to use a substance that dissolves a large amount of water, dissolves only a small amount of other components in the gas sample, and has a low solvent vapor pressure. In practice, methanol, ethanol,
Dimethylformamide etc. are used. Since it is necessary to make the solvent anhydrous with the KF reagent before measuring the moisture content, it is preferable that the solvent used has as little moisture as possible.
（効果）
本発明による気体試料中の水分オンライン分析装置の主
な利点は次の通りである。(Effects) The main advantages of the online analyzer for moisture in gas samples according to the present invention are as follows.
（１）従来分析できなかった高精度の気体試料中の水分
をオンラインで分析できる。(1) Moisture in gas samples can be analyzed online with high precision, which was previously impossible.
（２）液体試料中の水分を分析するカールフィッシャー
分析計を改造することにより１本発明の分析装置が得ら
れることから９水分析装置は気体試料および液体試料の
両者の分析ができる。(2) Since the analyzer of the present invention can be obtained by modifying a Karl Fischer analyzer that analyzes water in liquid samples, the water analyzer can analyze both gas samples and liquid samples.
（３）複数の気体試料採取用の電磁弁を設置し、切換え
る方式とすることにより、多流路の気体試料の水分分析
ができる。(3) Moisture analysis of gas samples in multiple channels can be performed by installing and switching a plurality of solenoid valves for gas sample collection.
（４）分析値を外部調節計への信号として出力すること
により、直接プロセス制御に用いて、蒸溜装置における
エネルギー節減を計ること等ができる。(4) By outputting the analysis value as a signal to an external controller, it can be used for direct process control, such as measuring energy savings in the distillation apparatus.
（実施例）
本発明による気体試料分析装置を用い、高純度水素製造
装置の製品水素中の水分測定を行った。(Example) Using the gas sample analyzer according to the present invention, water content in product hydrogen of a high-purity hydrogen production apparatus was measured.
第一図において滴定瓶２（容量０．３Ｌ）中の溶媒には
メタノール（水分０．０１％し以下）を用いカールフィ
ッシャー試薬で無水状態とした後、電磁弁１０より製品
水素を導入し、その通過量をガスメーター１３にて測定
した。In Figure 1, methanol (water content 0.01% or less) is used as the solvent in the titration bottle 2 (capacity 0.3 L), and after making it anhydrous with Karl Fischer reagent, product hydrogen is introduced from the solenoid valve 10. The amount of gas passing through was measured using a gas meter 13.
ガスメーターはＩＬ／１回転の湿式ガスメーターを使用
し、ガスメーターの文字盤に４個の充所プレートを取付
けそのパルス数により通過ガス量を測定した。製品水素
の純度は９９．９９９％以上が要求され、水分をｌｐｐ
ｍ以下に管理する必要がある。A wet gas meter with IL/1 rotation was used as the gas meter, and four filling plates were attached to the dial of the gas meter, and the amount of passing gas was measured by the number of pulses. The purity of the product hydrogen is required to be 99.999% or more, and the water content is reduced to lpp.
m or less.
各分析において、試料を約５０ＯＬ導入して分析した結
果、 Ｏ０ｌｐｐｍ以上の精度が得られ、この製品水素
中の水分を充分に管理することができた。In each analysis, about 50 OL of sample was introduced and analyzed, and as a result, an accuracy of 00 lppm or higher was obtained, and the water content in the product hydrogen could be adequately controlled.
第一図は本発明による気体試料中の水分のオンライン分
析計の構成図である。FIG. 1 is a block diagram of an online analyzer for moisture in a gas sample according to the present invention.
Claims (1)
ッシャー試薬で無水状態とした後、オンラインで気体試
料を吹き込み水分を吸収させ、当該吸収液中の水分をカ
ールフィッシャー試薬で滴定すると共に、吸収後の気体
試料をガスメーターに通過させて、当該ガスメーターの
指針の回転を光センサーで読み取るとることにより、気
体試料量を測定し、カールフィッシャー試薬の滴定によ
る水分量と気体試料量からの換算によって、気体試料中
の水分濃度を測定することを特徴とする気体試料中の水
分のオンライン分析装置After putting a water-soluble solvent into a sealed titration bottle and making it anhydrous with Karl Fischer reagent, a gas sample is blown on-line to absorb water, and the water in the absorption liquid is titrated with Karl Fischer reagent. The amount of gas sample is measured by passing the gas sample through a gas meter and reading the rotation of the pointer of the gas meter with an optical sensor, and then converting the amount of water from the titration of Karl Fischer reagent and the amount of gas sample. An online analyzer for moisture in a gas sample, which measures the moisture concentration in a gas sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61193968A JP2575662B2 (en) | 1986-08-21 | 1986-08-21 | On-line analyzer for moisture in gas samples |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61193968A JP2575662B2 (en) | 1986-08-21 | 1986-08-21 | On-line analyzer for moisture in gas samples |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6350751A true JPS6350751A (en) | 1988-03-03 |
| JP2575662B2 JP2575662B2 (en) | 1997-01-29 |
Family
ID=16316763
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61193968A Expired - Lifetime JP2575662B2 (en) | 1986-08-21 | 1986-08-21 | On-line analyzer for moisture in gas samples |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2575662B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61107492A (en) * | 1984-10-30 | 1986-05-26 | アマノ株式会社 | Patrol recorder |
| CN109100465A (en) * | 2017-06-21 | 2018-12-28 | 中国计量科学研究院 | A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5679852U (en) * | 1979-11-27 | 1981-06-29 |
-
1986
- 1986-08-21 JP JP61193968A patent/JP2575662B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5679852U (en) * | 1979-11-27 | 1981-06-29 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61107492A (en) * | 1984-10-30 | 1986-05-26 | アマノ株式会社 | Patrol recorder |
| CN109100465A (en) * | 2017-06-21 | 2018-12-28 | 中国计量科学研究院 | A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device |
| CN109100465B (en) * | 2017-06-21 | 2024-04-12 | 中国计量科学研究院 | Azeotropic distillation sampling device and moisture measurement system comprising same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2575662B2 (en) | 1997-01-29 |
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