JPS60219555A - Solvent for measuring moisture by karl fischer technique - Google Patents
Solvent for measuring moisture by karl fischer techniqueInfo
- Publication number
- JPS60219555A JPS60219555A JP7520484A JP7520484A JPS60219555A JP S60219555 A JPS60219555 A JP S60219555A JP 7520484 A JP7520484 A JP 7520484A JP 7520484 A JP7520484 A JP 7520484A JP S60219555 A JPS60219555 A JP S60219555A
- Authority
- JP
- Japan
- Prior art keywords
- methanol
- added
- karl fischer
- time
- 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.)
- Granted
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】
カールフィッシャー試薬は、含水物中の水とだけ反応す
るために水分の測定には最良の方法であるが、この試薬
と水との反応は試薬の成分であるヨード、亜硫酸ガスお
よびピリジンと溶媒の成分であるメタノールと被測定物
中の水との玉名の協奏反応といわれているので、反応次
数は少なくとも五次となり、終末点近くになると反応速
度は非常にゆるやかになって、測定時間が長くかかる欠
点がある。これをさけるために含水量より一定量の過剰
の試薬を加えた時点で滴下を止め(この時までの試薬の
使用量をAll11とする)、時間がたって過剰の試薬
が残存水分と反応して消滅した時、再び過剰の試薬を滴
下する(この時までの試薬の使用量をB mlとする)
。(B−Δ)mJの試薬が消費されるまでの待ち時間が
一定時間(1〜0゜5分)より越えた場合すなわち反応
速度が一定値より遅くなったときを終末点とする方法が
一般に用いられている。従って、前記五次反応の速度定
数を大にすれば測定時間は短縮される訳である。DETAILED DESCRIPTION OF THE INVENTION Karl Fischer reagent is the best method for measuring moisture because it reacts only with water in hydrated materials, but the reaction between this reagent and water is due to the presence of iodine, which is a component of the reagent. It is said to be a Tamana concerted reaction between sulfur dioxide gas, pyridine, methanol as a solvent component, and water in the sample to be measured, so the order of the reaction is at least fifth order, and the reaction rate becomes very slow near the end point. Therefore, there is a drawback that measurement time is long. To avoid this, stop dropping when a certain amount of excess reagent is added than the water content (the amount of reagent used up to this point is All11), and over time the excess reagent will react with the remaining water. When it disappears, drop the excess reagent again (the amount of reagent used up to this point is B ml)
. Generally, the end point is when the waiting time until (B-Δ) mJ of reagent is consumed exceeds a certain time (1 to 0°5 minutes), that is, when the reaction rate becomes slower than a certain value. It is used. Therefore, by increasing the rate constant of the fifth-order reaction, the measurement time can be shortened.
そこで、本発明者は1反応溶媒のメタノールにトリエチ
ルアミンを加えると、測定時間を大ijに短縮出来るこ
とを発見した。またトリエチルアミンは実施例に見られ
るように水分測定に悪影響を及ぼさない。本発明は5.
JrS水分のill’l定(カールフィッシャー法)に
おいて、滴定フラスコ中に入れる試料の溶媒に関するも
のである。、J I Sによると溶媒はカールフィッシ
ャー用メタノール約25m1を使用し、まず試料をこの
溶媒に溶かし1、カルフィッシャー試薬の適量を加えて
無水状態にする1次にカールフィッシャー試薬を滴下し
て待ち時間を30秒とし、滴下の始めから終末点まで到
るまでの時間は実施例1の水の添加量3 /j lの場
合について見ると7〜j2分間であるが、、JISのメ
タノールの替りに本発明の溶媒を用いるときは同し操作
で2分間以内となって、イ1り定時間が大11]に短縮
されて非フ:!に便利である。Therefore, the present inventor discovered that by adding triethylamine to methanol, which is one of the reaction solvents, the measurement time can be shortened by a large amount. Furthermore, triethylamine does not have an adverse effect on moisture measurement as seen in the examples. The present invention is 5.
This relates to the solvent of the sample placed in the titration flask in the ill'l determination of JrS water content (Karl Fischer method). According to JIS, the solvent used is about 25 ml of Karl Fischer methanol. First, dissolve the sample in this solvent 1. Add an appropriate amount of Kar Fischer reagent to make it anhydrous. Next, add Karl Fischer reagent dropwise and wait. When the time is 30 seconds, the time from the beginning of dropping to the end point is 7 to 2 minutes in the case of Example 1 where the amount of water added is 3/j l, but when using JIS methanol instead When using the solvent of the present invention, the same operation takes less than 2 minutes, which shortens the fixed time by as much as 11 times, making it a breeze! It is convenient for
実施例 1
.118カールフイツシヤー法の操作にならって、まず
メタノールを電極が全部ひたるまで入れるがこの時、ト
リエチルアミンをメタノールの1/。Example 1. 118 Following the Karl Fischer method, first add methanol until the electrode is fully submerged, and at this time add 1/1/2 of triethylamine to the amount of methanol.
容加える。次いで、カールフィッシャー試薬を加えて滴
定フラスコ内を無水の状態にする。次にマイクロシリン
ジを用いて純水3μl又はl Ou ]を加え、秒時訓
をりJかしてJISカールフィッシャー試薬を毎秒2〜
3滴の早さで加え、反応終了の待ち時間を30秒として
終末点適の時間を測定した結果と、溶媒として、J I
Sメタノール(カールフィッシャー川)を前記混合液
のかわりに使用した場合の測定結果とを比較すると次の
ようであった。尚、以下に掲げる実験データは同じ反応
溶媒に対し試薬を引続き加えて行った結果である。Add content. Next, Karl Fischer reagent is added to make the inside of the titration flask anhydrous. Next, add 3 μl or l Ou of pure water using a microsyringe, and add JIS Karl Fischer reagent every 2 to 10 seconds.
J I
A comparison with the measurement results obtained when S methanol (Karl Fischer River) was used instead of the above-mentioned liquid mixture revealed the following results. The experimental data listed below is the result of successive additions of reagents to the same reaction solvent.
従って、第一段の例で水分添加に;3μlのときの平均
所要時間は〕分28秒となり、これから待ち時間の30
秒を引いた58秒で試薬使用r11の平均0.88m1
(約!30滴)が/J[・されることになって。Therefore, in the first stage example, the average time required to add 3 μl of water is 1 minute and 28 seconds, and from this the waiting time of 30
The average of reagent usage r11 is 0.88ml in 58 seconds after subtracting the seconds.
(about! 30 drops) is to be /J[・.
これは毎秒1.5滴であるから殆ど連続滴下に近いli
tさでd111定が行オ〕れたことを示している。This is 1.5 drops per second, so it is almost continuous dripping.
This shows that the d111 constant was turned off at t.
実施例2 実施例Jと同様であるが、水の添加laを3
711にした場合だけについてメタノールと1ヘリエチ
ルアミンの比を表のようにして行った。Example 2 Same as Example J, but with water addition la of 3
The ratio of methanol to 1 heliethylamine was determined as shown in the table only for the case where 711 was used.
計1 メタノール対1−リエチルアミンの容暇比が16
:1以」−になると、41す定所要時間が2分を越える
ようになるので、1−リエチルアミンの76加効果が少
ない。Total 1 The ratio of methanol to 1-ethylamine is 16
:1 or more, the required time for 41 exceeds 2 minutes, so the effect of 76 addition of 1-ethylamine is small.
註2 メタノール対トリエチルアミンの容!+’<比が
1:4以下になろと、消1’したノJ−ルフィシャー1
拭薬が〆容体、中で分離づ−るので滴定不fIしてある
。Note 2: Methanol vs. triethylamine content! +'
Since the wipes separate in the container, titration is not performed.
特fl出願人 氏名 渡辺彦助Special fl applicant name: Hikosuke Watanabe
Claims (1)
量を越え3容量以下とよりなるカールフィッシャー法に
よる水分測定用の溶媒1 volume of methanol and '/1 volume of triethylamine. Solvent for moisture measurement by Karl Fischer method with a volume of more than 3 volumes or less
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7520484A JPS60219555A (en) | 1984-04-16 | 1984-04-16 | Solvent for measuring moisture by karl fischer technique |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7520484A JPS60219555A (en) | 1984-04-16 | 1984-04-16 | Solvent for measuring moisture by karl fischer technique |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS60219555A true JPS60219555A (en) | 1985-11-02 |
JPH0571906B2 JPH0571906B2 (en) | 1993-10-08 |
Family
ID=13569426
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP7520484A Granted JPS60219555A (en) | 1984-04-16 | 1984-04-16 | Solvent for measuring moisture by karl fischer technique |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS60219555A (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56147064A (en) * | 1980-03-19 | 1981-11-14 | Merck Patent Gmbh | Karl fisher's reagent containing no pyridine and water measurement employing same |
JPS58147650A (en) * | 1982-02-12 | 1983-09-02 | メルク・パテント・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング | Karl fischer reagent and method of measuring moisture by using said reagent |
-
1984
- 1984-04-16 JP JP7520484A patent/JPS60219555A/en active Granted
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56147064A (en) * | 1980-03-19 | 1981-11-14 | Merck Patent Gmbh | Karl fisher's reagent containing no pyridine and water measurement employing same |
JPS58147650A (en) * | 1982-02-12 | 1983-09-02 | メルク・パテント・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング | Karl fischer reagent and method of measuring moisture by using said reagent |
Also Published As
Publication number | Publication date |
---|---|
JPH0571906B2 (en) | 1993-10-08 |
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