JPS5866846A - Karl fischer's reagent - Google Patents
Karl fischer's reagentInfo
- Publication number
- JPS5866846A JPS5866846A JP16667481A JP16667481A JPS5866846A JP S5866846 A JPS5866846 A JP S5866846A JP 16667481 A JP16667481 A JP 16667481A JP 16667481 A JP16667481 A JP 16667481A JP S5866846 A JPS5866846 A JP S5866846A
- Authority
- JP
- Japan
- Prior art keywords
- reagent
- added
- pyrrolidone
- titration
- solvent
- 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
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/168—Determining water content by using Karl Fischer reagent
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はカール・フイシャー試薬に関するものであり、
特にコーピロリドンを溶媒とする二液用カール・フイシ
ャー試薬に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to Karl-Fischer reagents,
In particular, it relates to a two-component Karl-Fischer reagent using corpyrrolidone as a solvent.
カール・フイシャー試薬は、周知のように溶液中の水分
の測定に広く用いられており、微量の水分でも正確に測
定することができる。カール・フイシャー試薬には、そ
の成分である沃素、二酸化硫黄、ピリジンおよびメタノ
ールを単一の溶液中に含有させ九−原型試薬と、これら
を２つの別々の溶液中に分けて含有させた二液型試薬と
があり、そのいずれもが実用に供されている。As is well known, the Karl-Fischer reagent is widely used to measure water in solutions, and can accurately measure even trace amounts of water. The Karl-Fischer reagent contains the nine-prototype reagent, which contains its components iodine, sulfur dioxide, pyridine, and methanol in a single solution, and the two-part reagent, which contains these components separately in two separate solutions. There are two types of reagents, all of which are in practical use.
最近、臭気のあるピリジンの代りにジェタノールアミン
等を用いたカール争フイシャー試薬が提案されている。Recently, a Karl-Fischer reagent using jetanolamine or the like in place of the odorous pyridine has been proposed.
しかし、ジェタノールアミンを用いたー液型試薬は力価
が低下しやすいので、ジェタノールアミンおよび二酸硫
黄をメタノールに溶解した溶液（Ａ液）と、沃素をメタ
ノールに溶解した溶液（Ｂ液）とからなる二液型試薬も
提案されている。との二液型試薬は、従来のカール・フ
ィシャー試薬よりも水との反応速度が早いといわれてい
る。しかし、この試薬は、いずれの液もメタノールを溶
媒としているため、ケトンやアルデヒド等の水分の測定
に適用することは困難である。However, the titer of liquid-type reagents using jetanolamine tends to decrease, so a solution of jetanolamine and sulfur diacid dissolved in methanol (solution A) and a solution of iodine dissolved in methanol (solution B) are used. ) has also been proposed. The two-component reagent is said to have a faster reaction rate with water than the conventional Karl Fischer reagent. However, since all of these reagents use methanol as a solvent, it is difficult to apply them to the measurement of water content such as ketones and aldehydes.
本発明はコービロリドンと沃素を含む溶液からなる二液
用カール・フィシャー試薬を提供するものであり、この
試薬は、滴定溶媒を選択することにより、ケトンやアル
デヒド等の水分の測定にも適用することができる。The present invention provides a two-component Karl Fischer reagent consisting of a solution containing Corbyrolidone and iodine, and this reagent can also be applied to the measurement of water content of ketones, aldehydes, etc. by selecting the titration solvent. I can do it.
本発明についてさらに詳細に説明すると、本発明に係る
カール・フイシャー試薬は、基本的には、コーピロリド
ンに沃素を溶解することにより調製される。To explain the present invention in more detail, the Karl-Fischer reagent according to the present invention is basically prepared by dissolving iodine in copyrrolidone.
２−ピロリドンは沃素に対して大きな溶解力を有するの
で、１０■−ＨｔＯ／ｍ１以上の高力価の試薬でも容易
に調製することができる。捷だ、試薬は安定で、長期間
の保存に耐える。Since 2-pyrrolidone has a large dissolving power for iodine, it can be easily prepared even with a reagent with a high potency of 10 -HtO/ml or more. The reagents are stable and can be stored for long periods of time.
本発明に係る試薬には、さらに二酸化硫黄を含有させる
のが好ましい。二酸化硫黄を含む滴定溶媒を用いれば、
二酸化硫黄を含まない試薬でも水分の測定を行なうこと
は可能である。しかし試薬中に二酸化硫黄を含有させて
おけば、滴定溶媒中の二酸化硫黄の濃度を低下させるこ
とができる。二酸化硫黄は沃素に対し／ｊ倍モル以上含
有させる。特に２〜１０倍モルの二酸化硫黄を含有させ
るのが好ましい。メタノールと異なり、２−ピロリドン
は二酸化硫黄に対しても大き橙溶解力を有している。Preferably, the reagent according to the present invention further contains sulfur dioxide. If a titration solvent containing sulfur dioxide is used,
It is possible to measure moisture with reagents that do not contain sulfur dioxide. However, if sulfur dioxide is included in the reagent, the concentration of sulfur dioxide in the titration solvent can be reduced. Sulfur dioxide is contained in a molar amount of /j times or more relative to iodine. In particular, it is preferable to contain sulfur dioxide in an amount of 2 to 10 times the mole. Unlike methanol, 2-pyrrolidone also has a large orange-dissolving power for sulfur dioxide.
本発明に係るカール・フイシャー試薬は、所望により、
プロピレンカーボネートやクロロホルムなどの反応を妨
害しない他の溶媒を含有していてもよい。これらの溶媒
の含有量は任意であり、例えばコービロリドンにこれの
９倍（容量）のプロピレンカーボネートまだはクロロホ
ルムを加えた混合溶媒に、沃素と沃素に対して３倍モル
の二酸化硫黄を溶解させることにより試薬を調製するこ
とができる。The Karl-Fischer reagent according to the present invention may optionally include:
It may also contain other solvents that do not interfere with the reaction, such as propylene carbonate and chloroform. The content of these solvents is arbitrary; for example, iodine and 3 times the mole of sulfur dioxide relative to the iodine can be dissolved in a mixed solvent of Corbyrolidone, 9 times (volume) of propylene carbonate, and chloroform. The reagent can be prepared by
本発明に係るカール・フイシャー試薬を用いて試料中の
水分を測定するには、適当な滴定溶媒中に試料を入れ、
本発明に係るカール・フイシャー試薬で常法により滴定
すればよい。滴定溶媒としては、例えば特願昭５５−／
４１９９ に記載されているようなりロロホルムおよ
びアルキレンカーボネートを主体とし、さらにピリジン
、起さない試料の場合には、＆−／２チ（容量）のジェ
タノールアミンと２〜４Ｉ（容量）チの二酸化硫黄を含
むメタノール溶液を用いるのが好ましく、この溶液中で
は滴定反応がきわめてすみやかに進行する。寿お、本発
明に係る試薬が十分な量の二酸化硫黄を含んでいる場合
には二酸化硫黄を含まない滴定溶媒を用いることもでき
るが、二酸化硫黄を含む滴定溶媒を用いる方が反応の進
行が早いので好ましい。To measure the water content in a sample using the Karl-Fischer reagent according to the present invention, place the sample in a suitable titration solvent,
Titration may be carried out by a conventional method using the Karl-Fischer reagent according to the present invention. As a titration solvent, for example,
4199, consisting mainly of loloform and alkylene carbonate, and in the case of samples that do not contain pyridine, &-/2 t (by volume) of jetanolamine and 2 to 4 I (by volume) of dioxide. Preferably, a methanol solution containing sulfur is used, in which the titration reaction proceeds very rapidly. Toshio, if the reagent according to the present invention contains a sufficient amount of sulfur dioxide, a titration solvent that does not contain sulfur dioxide can be used, but the reaction progresses better when a titration solvent that contains sulfur dioxide is used. It's fast so it's preferable.
以下に実施例により本発明をさらに具体的に説明するが
、本発明はその要旨をこえない限り以下の実施例に限定
されるものではない。The present invention will be explained in more detail with reference to Examples below, but the present invention is not limited to the following Examples unless it exceeds the gist thereof.
実施例
２−ピロリドンに沃素２１．２ ｆおよび二酸化硫黄／
Ａ、Ｏｆを溶解し、さらに−一ビロリドンで全量をＳθ
ｏｍｌとした。この試薬の力価は！ 、！； Ｏｍｑ
Ｈ２０／ ｍｌであった。Example 2 - Pyrrolidone with 21.2 f of iodine and sulfur dioxide/
Dissolve A and Of, and further add -1 pyrrolidone to Sθ
oml. What is the potency of this reagent? ,! ; Omq
It was H20/ml.
メタノールにジェタノールアミンを溶解した混合溶媒に
二酸化硫黄ガスを吹込み、これをさラニメタノールで稀
釈して、メタノールｇ６（容！ ） ％ 、ジェタノー
ルアミン１０−、（容量）チ、二酸化硫黄亭（容量）チ
を含む滴定溶媒を調製した。Sulfur dioxide gas is blown into a mixed solvent in which jetanolamine is dissolved in methanol, and this is diluted with methanol to give methanol g6 (volume!) %, jetanolamine 10-, (volume) thi, sulfur dioxide (by volume) A titration solvent containing H was prepared.
この滴定溶媒Ｓθｍｌに試料を採取し、自動滴定装置（
ＭＣＩ ＭｏｖｗＬＫＦ−ｏｌ、三菱化成工業■製）を
用いて上記の試薬で滴定した。各試料について、同一の
滴定溶媒を用いてＳ回滴定を行につだ。結果を表に示す
。A sample was collected in this titration solvent Sθml, and an automatic titrator (
Titration was carried out with the above reagent using MCI MovwLKF-ol (manufactured by Mitsubishi Chemical Industries, Ltd.). For each sample, perform S titrations in a row using the same titration solvent. The results are shown in the table.
この結果から明らかなように、本発明に係るカール・フ
ィシャー試薬は機敏の水分でも極めて精度よく測定する
ことができる。As is clear from these results, the Karl Fischer reagent according to the present invention can measure even sensitive moisture with extremely high accuracy.
Claims (1)
カール・フイシャー試薬。 （２、特許請求の範囲第１項記載゛のカール・フイシャ
ー試薬において、該溶液がさらに二酸化硫黄を含有して
いることを特徴とするもの。 （３）特許請求の範囲第１項または第２項記載のカール
・フイシャー試薬において、該溶液がさらに他の溶媒を
含有していることを特徴とするもの。[Scope of Claims] (1) A two-part Karl-Fischer reagent consisting of a solution containing 2-pyrrolid/and iodine. (2. The Karl-Fischer reagent according to claim 1, characterized in that the solution further contains sulfur dioxide. (3) Claim 1 or 2 3. The Karl-Fischer reagent according to section 1, characterized in that the solution further contains another solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16667481A JPS5866846A (en) | 1981-10-19 | 1981-10-19 | Karl fischer's reagent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16667481A JPS5866846A (en) | 1981-10-19 | 1981-10-19 | Karl fischer's reagent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5866846A true JPS5866846A (en) | 1983-04-21 |
Family
ID=15835615
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16667481A Pending JPS5866846A (en) | 1981-10-19 | 1981-10-19 | Karl fischer's reagent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5866846A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6140732A (en) * | 1998-04-08 | 2000-10-31 | Mitsubishi Denki Kabushiki Kaisha | Armature coil conductor and method of manufacture therefor |
-
1981
- 1981-10-19 JP JP16667481A patent/JPS5866846A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6140732A (en) * | 1998-04-08 | 2000-10-31 | Mitsubishi Denki Kabushiki Kaisha | Armature coil conductor and method of manufacture therefor |
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