JPS6082860A - Titration reagent for moisture measurement - Google Patents
Titration reagent for moisture measurementInfo
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- JPS6082860A JPS6082860A JP19126083A JP19126083A JPS6082860A JP S6082860 A JPS6082860 A JP S6082860A JP 19126083 A JP19126083 A JP 19126083A JP 19126083 A JP19126083 A JP 19126083A JP S6082860 A JPS6082860 A JP S6082860A
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- alkyl group
- amine
- alkyl
- hydrogen atom
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Classifications
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- 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
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- 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】 本発明は水分測定用滴定試薬に関1−るものである。[Detailed description of the invention] The present invention relates to a titration reagent for measuring moisture content.
従来、溶液中の水分の測定は原理的にKarlFisc
herによって見つけられたカール・フィッシャー反応
を利用して行なわれてきた。Conventionally, the measurement of water in a solution is based on the principle of Karl Fisc.
It has been carried out using the Karl Fischer reaction discovered by Herr.
そして、二酸化硫黄、ヨウ素及びピリジンを主成分とし
て含み、それらをメタノール等の溶媒に溶かしたもの等
がカール・フインヤー試薬として実用化されており、こ
の場合のカール・フイシャー試薬と水との反応は次式の
如く進行する。A substance containing sulfur dioxide, iodine, and pyridine as main components and dissolved in a solvent such as methanol has been put into practical use as a Karl-Fuyscher reagent. In this case, the reaction between the Karl-Fuyscher reagent and water is The process proceeds as shown in the following equation.
so2+工2 +H20+305H5N−コc、、u5
N・H工+05H5N・SOs・・・(1)05H5N
−BOs+0H80H−0,H5N−H8O40H8・
・・・・・・・・・・・(2)また、水分測定の手法と
しては上記のような、カール・フイシャー試薬をそのま
ま水と定量的に反応させて、水分量を測定する容量滴定
法の他に上記カール・フイシャー反応に必要なヨウ素を
ヨウ素化物イオンの電解酸化により内部的に生成させて
水分を測定する電層滴定法がある。so2 + engineering 2 +H20+305H5N-ko c,,u5
N/H engineering +05H5N/SOs...(1)05H5N
-BOs+0H80H-0,H5N-H8O40H8・
・・・・・・・・・・・・(2) Also, as a method for measuring moisture, volumetric titration method, which quantitatively reacts the Karl-Fischer reagent as it is with water to measure the moisture content, as mentioned above, is used. In addition, there is an electrostatic titration method in which the iodine required for the Karl-Fischer reaction is internally generated by electrolytic oxidation of iodide ions and water is measured.
また上記した容量滴足法による水分測定に用いろカール
・フイシャー試薬には、二酸化硫黄、ヨウ素及びピリジ
ン等の各成分を単一の溶液中に含有させたー液型試薬の
他に、ヨウ素を適当な溶媒に溶解したものを滴足剤とし
、二酸化硫黄及びピリジン等を適当な溶媒に溶角了した
ものを溶剤として用いろ二液型試薬がある。In addition, the Karl-Fischer reagent used for moisture measurement by the above-mentioned volumetric dropping method contains components such as sulfur dioxide, iodine, and pyridine in a single solution. There are two-component reagents that are dissolved in an appropriate solvent as a droplet and sulfur dioxide, pyridine, etc. dissolved in an appropriate solvent as a solvent.
特に、二液型試薬は、測定の妨害が少なく、また測定時
間が短かい利点がある。In particular, two-component reagents have the advantage of causing less interference with measurements and shortening the measurement time.
最近、ピリジンの特異な臭いをきらって電量滴定試薬及
び容量満足試薬に於てピリジンの代シにイミダゾールや
ジェタノールアミンなトラ用いた滴定試薬が提案され、
ピリジン以外のアミンを用いた水分測定用滴定試薬の可
能性が示唆された(特開昭!;t−t372jO号公報
参照)。Recently, due to the peculiar odor of pyridine, titration reagents using imidazole or jetanolamine as a substitute for pyridine in coulometric titration reagents and volumetric reagents have been proposed.
The possibility of a titration reagent for measuring water content using an amine other than pyridine has been suggested (see Japanese Patent Application Laid-open No. Sho!; t-t372jO).
しかしながら、これらはピリジンより反応性に富むため
水分測定の精度が低下したり測定が不能であったシする
場合があシその改良が望まれていた。However, since these are more reactive than pyridine, the accuracy of moisture measurement may be lowered or measurement may be impossible, and an improvement has been desired.
本発明者らは以上の事実に基づき従来操作上不便をきた
していたその特有な臭いのしないカール・フインヤー試
薬を見いだすべく鋭意検討した結果、本発明に到達した
。Based on the above-mentioned facts, the present inventors conducted intensive studies to find a Karl-Fyer reagent that does not have the characteristic odor that has conventionally caused operational inconvenience, and as a result, the present invention was achieved.
即ち、本発明は、ヨウ素又はヨウ素化物、二酸化硫黄並
びに下記(イ)、(ロ)、←→及びに)がら成ろ群から
選ばれろ少なくとも7種のアミンを含有してなる水分測
定用滴定試薬
(イ)一般式 CLNR1R2(式中、R1及びR2は
水素原子、アルキル基、隣接1−ろl(原子と共に閉環
してもよいアルキレン基−ピリジル基又はピロリジニル
基である)で表わされるアミン。That is, the present invention provides a titration reagent for measuring moisture content, which contains iodine or an iodide, sulfur dioxide, and at least seven amines selected from the group consisting of (a), (b), ←→, and (b) below. (a) An amine represented by the general formula CLNR1R2 (wherein R1 and R2 are a hydrogen atom, an alkyl group, or an adjacent 1-rolyne group (which may be a pyridyl group or a pyrrolidinyl group that may be ring-closed together with the atom).
(ロ) 一般式 R3→コトR4(式中、R8及びR4
は、水素原子、水酸基で置換されていてもよいアルキル
基、又は0nH2nOR(n ’= / 〜3、Rはア
ルキル基を表わ′1″)で示されろアルコキシアルキル
基であり R3及びR4が同時に水素原子であることは
ない)で表わされるアミン。(b) General formula R3 → R4 (in the formula, R8 and R4
is a hydrogen atom, an alkyl group optionally substituted with a hydroxyl group, or an alkoxyalkyl group represented by 0nH2nOR (n'=/~3, R represents an alkyl group '1''), and R3 and R4 are amines (which cannot be both hydrogen atoms at the same time).
’NR5R’
(ハ)一般式 e、R7(式中、R5、R6及びR7は
、水素原子又はアルキル基である)で表わされろアミン
。'NR5R' (c) An amine represented by the general formula e, R7 (wherein R5, R6 and R7 are hydrogen atoms or alkyl groups).
水素原子、アルキル基、0nH2nON (n = t
−3)で示されろシアン化アルキル基又はアルコキシ
カルボニルアルキル基であに’ 、R’、R9及びRl
Gが同時に水素原子であることはない)で表わされるア
ミン。Hydrogen atom, alkyl group, 0nH2nON (n = t
-3) is an alkyl cyanide group or an alkoxycarbonyl alkyl group represented by ', R', R9 and Rl
G is not a hydrogen atom at the same time).
及び、二酸化硫黄及びアミンを含有する溶液人並びにヨ
ウ素を含有する溶液Bから成る滴定試薬において、該溶
液A中のアミンが下記(イ)、(ロ)、(ハ)及びに)
から成る群から選ばnる少なくとも7種のアミンを含有
してなる水分測定用滴定試薬(イ)一般式 〇トNR’
R2(式中、R1及びR2は水素原子、アルキル基、隣
接するNJjA子と共に閉環していてもよいアルキレン
基、ピリジル基又はピロリジニル基である)で表わされ
ろアミン。And, in a titration reagent consisting of a solution containing sulfur dioxide and an amine and a solution B containing iodine, the amine in the solution A is as follows (a), (b), (c) and)
A titration reagent for moisture measurement containing at least seven amines selected from the group consisting of (a) General formula:
An amine represented by R2 (wherein R1 and R2 are a hydrogen atom, an alkyl group, an alkylene group which may be ring-closed with the adjacent NJjA atom, a pyridyl group, or a pyrrolidinyl group).
(ロ) 一般式 R3唖〉R4(式中、R3及びR4は
水素原子、水酸基で置換されていてもよいアルキル基、
又はC!nH2nOR(n = / −3、Rはアルキ
ルMを7わす)で示されろアルコキシアルキル基であり
、 R3及びR4が同時に水素原子であることはない
)で表わされろアミン。(b) General formula R3〉R4 (wherein R3 and R4 are a hydrogen atom, an alkyl group optionally substituted with a hydroxyl group,
Or C! An amine represented by nH2nOR (n = / -3, R is an alkoxyalkyl group, where R is 7 less than alkyl M, and R3 and R4 are never hydrogen atoms at the same time).
水素原子又はアルキル基である)で表わされ水素原子、
アルキル基、0nHznC!N (n =−i 〜3
)で示されるシアン化アルキル基又はアルコキンカルボ
ニルアルキル基であり、R8、R9及びRIGが同時に
水素原子であることはない)で表わされるアミン。a hydrogen atom or an alkyl group);
Alkyl group, 0nHznC! N (n = -i ~ 3
), and R8, R9 and RIG are not hydrogen atoms at the same time.
を要旨とするものである。The main points are as follows.
以下に、本発明につき、更に詳細に説明する。The present invention will be explained in more detail below.
本発明の水分測定用滴定試薬は、容量滴定、電量滴定の
いずれの滴定試薬としても好適に用いることができ、ま
た−液型試薬としてだけでなく、二液型試薬としても使
用できろものである。The titration reagent for moisture measurement of the present invention can be suitably used as a titration reagent for both volumetric titration and coulometric titration, and can also be used not only as a liquid type reagent but also as a two-liquid type reagent. be.
本発明の水分測定用滴定試薬はヨウ素又はヨウ素化物、
二酸化硫黄及び特定のアミンを含有することが必要であ
る。The titration reagent for moisture measurement of the present invention includes iodine or iodide,
It is necessary to contain sulfur dioxide and certain amines.
本発明の水分測定用滴定試薬を一液型試薬として用いろ
場合には、ヨウ素成分として、ヨウ素又はヨウ素化物を
、また、二液型試薬として用いる場合にはヨウ素を含有
させる。When the titration reagent for moisture measurement of the present invention is used as a one-component reagent, it contains iodine or an iodide as the iodine component, and when it is used as a two-component reagent, it contains iodine.
従って、通常はヨウ素(単体)が用いられるも、水分測
定する試料を注入する直前に全てヨウ素化物イオンとし
て存在させるので、滴定方法によってヨウ素又はヨウ素
化物を適宜用いればよい。Therefore, although iodine (single substance) is usually used, since all of the ions are made to exist as iodide ions just before injecting the sample to be measured for moisture content, iodine or iodide may be used as appropriate depending on the titration method.
ヨウ素化物としては、例えば、テトラブチルアンモニウ
ムアイオダイド船が挙げられろ。Examples of iodides include tetrabutylammonium iodide.
ヨウ素又はヨウ素化物の濃度は、ヨウ素化物イオンとし
て0.01〜θ、りmo]、//! 好ましくはo、
o 3〜o、 t o mo1/lの範囲である。一般
に、電量滴定試薬において、ヨウ素化物イオンの濃度が
高すぎろと反応速度が遅くなり、また、低すぎると電流
効率が低くなる傾向があるので、ヨウ素化物は、この濃
度範囲で含有させろ。The concentration of iodine or iodide is 0.01 to θ, as iodide ions, //! Preferably o,
The range is from o3 to o, to mo1/l. Generally, in a coulometric titration reagent, if the concentration of iodide ions is too high, the reaction rate will be slow, and if it is too low, the current efficiency will tend to decrease, so the iodide should be contained within this concentration range.
次に、二酸化硫黄は、反応を促進ずろ作用を有し、過剰
に存在させろことも可能である。しかしながら通常は0
.3〜.2mol/7の範囲、特にo、t〜/、J’m
Q’1μの範囲で包有させるのが好ましい。Next, sulfur dioxide has a reaction-promoting effect and can be present in excess. However, usually 0
.. 3~. in the range of 2 mol/7, especially o, t~/, J'm
It is preferable to include it in the range of Q'1μ.
また、不発明の水分測定用i的足試薬は以TK述べる特
定のアミンを含有する。Additionally, the uninvented idiopathic reagent for moisture determination contains specific amines as described below.
即ち、下記(イ)、仲)、←う及び(に)から成る群か
ら選ばれる少なくともl釉のアミンを含有づ−る。That is, the glaze contains at least one amine selected from the group consisting of (A), (N), (U) and (N) below.
(’fl 一般式c)−NR’I?2(式中、R’ 及
U B21d−水素原子、アルキル基、隣接するlJ原
子と共に閉環していてもよいアルキレン基、ピリジル基
又はピロリジニル基である)で表わされるアミン。('fl General formula c)-NR'I? 2 (wherein R' and U B21d- are a hydrogen atom, an alkyl group, an alkylene group which may be ring-closed together with the adjacent lJ atom, a pyridyl group or a pyrrolidinyl group).
素原子、水酸基で置換されていてもよいアルキル基、又
は0nHznOR(n = / 〜3、Rはアルキル基
を表わf)で示されるアルコキンアルキル基であり 、
”3及びR4が同時に水素原子であることはない)で表
わされろアミン。An elementary atom, an alkyl group optionally substituted with a hydroxyl group, or an alkoxyalkyl group represented by 0nHznOR (n = / ~ 3, R represents an alkyl group and f),
``3 and R4 are never hydrogen atoms at the same time.''
R5R6 水素原子又はアルキル基である)で表わされるアミン。R5R6 An amine represented by a hydrogen atom or an alkyl group.
水素原子、アルキル基、cnH2nON (n = t
〜3 )で示さnるシアン化アルキル基又はアルコキ
シカルボニルアルキル基であ、Q、R8,R’及びR1
0が同時に水素原子であることはない)で表わされろア
ミン。Hydrogen atom, alkyl group, cnH2nON (n = t
~3) is a cyanated alkyl group or alkoxycarbonylalkyl group represented by n, and Q, R8, R' and R1
0 is not a hydrogen atom at the same time).
前記(イ)に分類さtl、ろアミンにおいてR1及びR
2は、水素原子、アルキル基、隣接するN原子と共に閉
環していてもよいアルキレン基、ピリジル基又はピロリ
ジニル基であるが、この中で、アルキル基としては炭素
数t−IIのアルキル基が好適である。R1 and R in tl and roamine classified as (a) above
2 is a hydrogen atom, an alkyl group, an alkylene group which may be ring-closed together with an adjacent N atom, a pyridyl group or a pyrrolidinyl group, and among these, an alkyl group having a carbon number of t-II is preferable as the alkyl group. It is.
具体的には、!−メチルアミノピリジン、λ−ジメチル
アミノピリジン、ゲージメチルアミノピリジン、グーピ
ロリジニルピリジン、λ、2′−ジピリジルアミンなど
が挙げられろ。in particular,! -methylaminopyridine, λ-dimethylaminopyridine, gauge methylaminopyridine, goupyrrolidinylpyridine, λ,2'-dipyridylamine, and the like.
以上の中でも特に、λ−ジメチルアミノピリジン、ゲー
ジメチルアミノピリジンを使用1ろことが好せしい。Among the above, it is particularly preferable to use λ-dimethylaminopyridine and gauge methylaminopyridine.
(ロ)に分類さ几ろアミンにおいて、R3及びR4は前
記したとおりであるが、その中で、水酸基で置換されて
いてもよいアルキル基としては特に水酸基で置換されて
いてもよい炭素数7−≠のアルキル基が好1しく、また
、CnH2noR(n=l〜3)で示さnろものとして
はRが炭素数/〜グのアルキル基、特にメチル基又はエ
チル基であるものが好適に用いられろ。In the amines classified as (b), R3 and R4 are as described above, but among them, the alkyl group which may be substituted with a hydroxyl group has particularly 7 carbon atoms which may be substituted with a hydroxyl group. An alkyl group in which -≠ is preferable, and an alkyl group in which R is represented by CnH2noR (n=1 to 3) is preferably an alkyl group having a carbon number of 1 to 3, particularly a methyl group or an ethyl group. Be used.
具体的には、1−ピリジンエタノール、λ−ピリジンプ
ロパノール、!、乙−ピリジンジメタツール、λ−メト
キンエチルピリジンなどが挙げられる。Specifically, 1-pyridine ethanol, λ-pyridine propanol,! , Otsu-pyridine dimetatool, λ-methquinethylpyridine, and the like.
以上の中でも特に−一ビリジンエタノールを使用するこ
とが好ましい。Among the above, it is particularly preferable to use -1-pyridine ethanol.
k−1に分類されろアミンにおいて、R5、R6及びR
7は前記したとお9であるが、その中で、アルキル基と
しては炭素数/〜グのものが好ましい。In amines classified as k-1, R5, R6 and R
7 is 9 as described above, and among these, as the alkyl group, those having carbon number/~g are preferable.
具体的には、N、N−ジエチル7−”)7、N 、 N
−ジプチルアニリン、 N、N−ジエチル−m−)ルイ
ジン等が挙げられろ。Specifically, N,N-diethyl 7-'')7,N,N
-diptylaniline, N,N-diethyl-m-)luidine, etc.
に)に分類されろアミンとしては、具体的には、3.3
′−イミノジプロピオニトリル、イミノジ酢酸ジエチル
、3−ジメチルアミノプロピオニトリルなどがある。Specifically, amines classified as 3.3
'-Iminodipropionitrile, diethyl iminodiacetate, 3-dimethylaminopropionitrile and the like.
−と−
以中の中でも特に、 3.3’−イミノジプロピオニト
リルを使用することが好ましい。-and- Among these, it is particularly preferable to use 3,3'-iminodipropionitrile.
上述したアミンの濃度は、二酸化硫黄に対するモル比で
0.3/l〜3/11特に0.7//〜+2//の割合
で含有させろことが好ましい。The concentration of the above-mentioned amine is preferably contained in a molar ratio of 0.3/l to 3/11, particularly 0.7// to +2// to sulfur dioxide.
上記した、ヨウ素又はヨウ素化物、二酸化硫黄及びアミ
ンの各成分は通常、カール・フインヤー試薬において一
般的に使用されている、メタノール、エタノール、イソ
プロパツール、メチルセロソルブ、クロロホルム、四塩
化炭素などの溶媒又はこれらの混合溶媒に前述した濃度
範囲で溶解させて水分測定用試薬と′1−ろ。The iodine or iodide, sulfur dioxide, and amine components listed above are typically solvents such as methanol, ethanol, isopropanol, methyl cellosolve, chloroform, and carbon tetrachloride, which are commonly used in Karl-Fyer reagents. Alternatively, it is dissolved in a mixed solvent of these in the concentration range mentioned above and used as a reagent for measuring moisture content.
また、二液型試薬においては、前記した二酸化硫黄及び
アミンを含有する浴液A(溶剤)と、ヨウ素を含有jる
溶液B(滴定剤)とに分けておくものの、−液量試薬と
不質的な差異はないので、前記した二酸化硫黄及びアミ
ンと、ヨウ素とを前述した濃度範囲で夫々上記した溶媒
中に溶解させておけばよい。In addition, in the case of a two-component reagent, although it is separated into the bath solution A (solvent) containing sulfur dioxide and amine and the solution B (titrant) containing iodine, the -liquid volume reagent and the liquid volume reagent are separated. Since there is no qualitative difference, the above-mentioned sulfur dioxide and amine, and iodine may be dissolved in the above-mentioned solvents respectively in the above-mentioned concentration ranges.
以下に実施例により本発明を更に具体的に説明するが、
本発明はその要旨を超えない限p以下の実施例によって
限定さnるものではない。The present invention will be explained in more detail with reference to Examples below.
The present invention is not limited to the following examples as long as they do not exceed the gist of the invention.
実施例−/〜4t(電量滴定用の一液型試薬)ヨウ素O
1t≠2を3M二酸化硫黄/メタノール溶液311rt
tlに溶解後水冷し、この溶液に、表−/ Vc示すア
ミンを表−7に示す添加量で夫々添加し、更にクロロホ
ルム2.tmlを加えた後メタノールで100m1とし
、滴定試薬を調製した。Example -/~4t (one-component reagent for coulometric titration) Iodine O
1t≠2 in 3M sulfur dioxide/methanol solution 311rt
After dissolving in Tl and cooling with water, the amines shown in Table-/Vc were added to this solution in the amounts shown in Table-7, and chloroform 2. After adding tml, the volume was made up to 100ml with methanol to prepare a titration reagent.
市販のカール・フイシャー電量滴?装置(ディジタル微
量水分測定装置OA〜02、三菱化成工業■社製)の陽
極室に得られた溶液の全量を入れ、陰極室には二酸化硫
黄/M及びμmmジメチルアミノビ99フフ、フを含有
したメタノール溶液と四塩化炭素のび:lの混合溶液を
入れた。Commercially available Karl Fischer coulometric drops? The entire amount of the obtained solution was put into the anode chamber of the device (digital trace moisture measuring device OA~02, manufactured by Mitsubishi Kasei Corporation), and the cathode chamber contained sulfur dioxide/M and μmm dimethylaminobi 99fu, Fu. A mixed solution of the methanol solution and 1:1 of carbon tetrachloride was added.
被水分測定試料として表−7に示す添加量の水を添加し
て上記電量滴定装置Ω操作法に従って水分測定を行なっ
た。結果を表−7に示す。Water in the amount shown in Table 7 was added as a sample to be measured for moisture content, and the water content was measured according to the coulometric titration Ω operating method. The results are shown in Table-7.
実施例−j〜7(容量満足用の二液型試薬)3M二酸化
硫黄/メタノール溶液3≠−を水冷しながら表−1に示
すアミンを表−/に示す添加量で夫々添加し、メタノー
ルで100rttlとした(溶液A)。ヨウ素、23t
をメタノール500WII!に溶解したものを溶液Bと
した。市販の容量滴定装置(カール・フインヤー自動滴
定装置KF−θ/三菱化成工業■社製)の満足容器に上
記溶液AをsOmJ入れ被水分測?試料として水を表−
7に示す添加量で添加して溶液Bで上記装置の操作法に
従って水分測定を行なった。Examples-j to 7 (Two-component reagent for satisfying capacity) While cooling a 3M sulfur dioxide/methanol solution 3≠- with water, the amines shown in Table-1 were added in the amounts shown in Table-/, and the mixture was diluted with methanol. 100 rttl (solution A). Iodine, 23t
Methanol 500WII! Solution B was obtained by dissolving the solution in The above solution A was poured in sOmJ into the container of a commercially available volumetric titrator (Karl Feynja automatic titrator KF-θ/manufactured by Mitsubishi Chemical Corporation) to measure water content. Take water as a sample.
The water content of solution B was measured in accordance with the operating method of the above-mentioned apparatus.
結果を表−7に示す。The results are shown in Table-7.
実施例−g
被水分測定試料として水の代わりに一足量のカーボネー
ト系化合物を添加して、その水分量を測定した以外、実
施例−7と同様にして水分測定を行なった。水分測定を
5回繰返し、その平均値を結果として表−2に示す。Example-g Moisture measurement was carried out in the same manner as in Example-7, except that instead of water, one foot of a carbonate-based compound was added as a moisture measurement sample and the moisture content was measured. The moisture measurement was repeated five times, and the average value is shown in Table 2.
比較例−l
ピリジンを含む市販のカール・フインヤー試薬アクアミ
クロンA(三菱化成工業−社製)を滴定試薬とした以外
は実施例−gと同様の操作で同一のカーボネート系化合
物の同量に含着れろ水分量を測定した。水分i!tll
7yLを5回繰返し、その平均値を結果として表−,
2に示す。Comparative Example-l The same amount of the same carbonate-based compound was mixed with the same amount of the same carbonate compound in the same manner as in Example-g, except that the commercially available Karl-Feyer reagent Aquamicron A (manufactured by Mitsubishi Chemical Industries, Ltd.) containing pyridine was used as the titration reagent. We measured the moisture content. Moisture i! tll
7yL is repeated 5 times and the average value is shown in the table below.
Shown in 2.
比較例−λ
イミダゾールを含む市販のカール・フインヤー試薬り−
ロマートA(リーデル・デ・ヘーン社fA)を滴定試薬
とした以外は、比較#/と同様にして水分測定を行なっ
几。結果を表−−2rK−示す。Comparative Example - Commercially available Karl-Fyer reagent containing λ imidazole -
Moisture measurement was carried out in the same manner as Comparison #/, except that Romato A (Riedel de Haene fA) was used as the titration reagent. The results are shown in Table 2rK.
表−ノ 出 願 人 三菱化成工業株式会社 代 理 人 弁理士 長谷用 − ほか/名Table-no Sender: Mitsubishi Chemical Industries, Ltd. Representative Patent Attorney Hase - Others/names
Claims (3)
(イ)、(ロ)、(ハ)及びに)から成る群から選ばれ
る少なくとも1種のアミンを含有してなる水分測定用滴
定試薬 水素原子、アルキル基、隣接するN原子と共に閉環して
いてもよいアルキレン基、ピリジル基又はピロリジニル
基である)で表わされるアミン。 (ロ) 一般式 RζζテR4(式中、R3及びR4は
水素原子、水酸基で置換されていてもよいアルキル基、
又は0nH2nOR(n = / 〜3、只はアルキル
基な表わす)で示されるアルコキンアルキル基であシ、
R3及びR4が同時に水素原子であることはない)で表
わされろアミン。 は、水素原子又はアルキル基である)で表わされるアミ
ン。 は水xi子、アルキル基、C!nHznON (n =
l〜3)で示されるシアン化アルキル基又はアルコキン
カルボニルアルキル基であり、R8、R9及びRIoが
同時に水素原子であることはない)で表わされろアミン
。(1) A hydrogen atom titration reagent for measuring moisture content, which contains iodine or an iodide, sulfur dioxide, and at least one amine selected from the group consisting of (a), (b), (c), and (d) below; An amine represented by an alkyl group, an alkylene group which may be ring-closed together with an adjacent N atom, a pyridyl group or a pyrrolidinyl group. (b) General formula RζζteR4 (wherein R3 and R4 are a hydrogen atom, an alkyl group optionally substituted with a hydroxyl group,
or an alkoxyalkyl group represented by 0nH2nOR (n = / ~ 3, the suffix represents an alkyl group),
R3 and R4 are not hydrogen atoms at the same time). is a hydrogen atom or an alkyl group). is water, alkyl group, C! nHznON (n =
An amine which is an alkyl cyanide group or an alkoxycarbonyl alkyl group represented by 1 to 3) in which R8, R9 and RIo are not hydrogen atoms at the same time.
ウ素を含有する溶液Bがら成る滴定試薬において、該溶
液A中のアミンが下記(イ)、(ロ)、H及びに)から
成る群から選ばれろ少なくとも1種のアミンを含有して
なる水分測定用滴定試薬 水素原子、アルキル基、@接するN原子と共に閉環して
いてもよいアルキレン基、ピリジル基又はピロリジニル
基である)で表わされるアミン。 (ロ)一般式 R8−(ぶトR4(式中、R8及びR4
は水素原子、水酸基で置換されていてもよいアルキル基
、又は0nHznOR(n = / 〜3、Rはアルキ
ル基を表わす)で示されろアルコキンアルキル基であシ
、R3及びR4が同時に水素原子であることはない)で
表わされるは、水素原子又はアルキル基であ7))で表
わされろアミン。 は水素原子、アルキル基、C+nH2nON (n =
l〜3)で示されるシアン化アルキル基又はアルコキシ
カルボニルアルキル基であり、R8、R9及びRIDが
同時に水素原子であることはない)で表わされるアミン
。(2) In a titration reagent consisting of a solution A containing sulfur dioxide and an amine and a solution B containing iodine, the amine in the solution A is selected from the group consisting of the following (a), (b), H, and (2). A titration reagent for measuring moisture content containing at least one amine.An amine represented by a hydrogen atom, an alkyl group, an alkylene group which may be ring-closed together with an adjacent N atom, a pyridyl group or a pyrrolidinyl group. (b) General formula R8-(butoR4 (in the formula, R8 and R4
is a hydrogen atom, an alkyl group optionally substituted with a hydroxyl group, or an alkoxyalkyl group represented by 0nHznOR (n = / ~ 3, R represents an alkyl group), and R3 and R4 are hydrogen atoms at the same time. 7) is a hydrogen atom or an alkyl group, and 7) is an amine. is a hydrogen atom, an alkyl group, C+nH2nON (n =
An amine represented by an alkyl cyanide group or an alkoxycarbonyl alkyl group represented by 1 to 3), in which R8, R9 and RID are not hydrogen atoms at the same time.
l〜3/lの範囲にあることを特徴とする特許請求の範
囲第1項または第2項に記載の水分測定用滴定試薬。(3) The molar ratio of amine to sulfur dioxide is 0.3/
The titration reagent for moisture measurement according to claim 1 or 2, characterized in that the titration reagent is in the range of 1 to 3/l.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19126083A JPS6082860A (en) | 1983-10-13 | 1983-10-13 | Titration reagent for moisture measurement |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP19126083A JPS6082860A (en) | 1983-10-13 | 1983-10-13 | Titration reagent for moisture measurement |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6082860A true JPS6082860A (en) | 1985-05-11 |
JPH0445782B2 JPH0445782B2 (en) | 1992-07-27 |
Family
ID=16271572
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP19126083A Granted JPS6082860A (en) | 1983-10-13 | 1983-10-13 | Titration reagent for moisture measurement |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6082860A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4851352A (en) * | 1985-06-15 | 1989-07-25 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Solvent composition for the determination of water by the Karl Fischer method |
Citations (1)
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 |
-
1983
- 1983-10-13 JP JP19126083A patent/JPS6082860A/en active Granted
Patent Citations (1)
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 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4851352A (en) * | 1985-06-15 | 1989-07-25 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Solvent composition for the determination of water by the Karl Fischer method |
Also Published As
Publication number | Publication date |
---|---|
JPH0445782B2 (en) | 1992-07-27 |
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