DE1086918B - Method for coulometric water determination - Google Patents

Method for coulometric water determination

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Publication number
DE1086918B
DE1086918B DEO6157A DEO0006157A DE1086918B DE 1086918 B DE1086918 B DE 1086918B DE O6157 A DEO6157 A DE O6157A DE O0006157 A DEO0006157 A DE O0006157A DE 1086918 B DE1086918 B DE 1086918B
Authority
DE
Germany
Prior art keywords
water
water determination
fischer
iodine
coulometric
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
Application number
DEO6157A
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German (de)
Inventor
Dipl-Chem Friedrich Oehme
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
FRIEDRICH OEHME DIPL CHEM
Original Assignee
FRIEDRICH OEHME DIPL CHEM
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by FRIEDRICH OEHME DIPL CHEM filed Critical FRIEDRICH OEHME DIPL CHEM
Priority to DEO6157A priority Critical patent/DE1086918B/en
Publication of DE1086918B publication Critical patent/DE1086918B/en
Pending legal-status Critical Current

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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

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  • 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)

Description

Verfahren zur coulometrischen Wasserbestimmung Bestimmungen kleiner Wassergehalte (Feinwasserbestimmungen) können bekanntlich mit gutem Erfolg nach der Karl-Fischer-Methode durchgeführt werden.Procedure for coulometric water determination Small determinations As is well known, water contents (fine water determinations) can be used with good success the Karl Fischer method.

Das Verfahren zeichnet sich durch die Anwendung eines Spezialreagenzes aus, welches titrimetrisch zur vorgelegten wasserhaltigen Probe zugegeben wird.The process is characterized by the use of a special reagent from which is added titrimetrically to the submitted water-containing sample.

Der Endpunkt der Titration kann dabei optisch oder elektrisch bestimmt werden.The end point of the titration can be determined optically or electrically will.

Bei sehr kleinen Wassergehalten ist die Fischer-Methode durch das unvermeidliche Einschleppen kleiner Wassermengen aus der feuchten Raumluft, durch die Notwendigkeit, die Fischer-Lösung zu verdünnen und durch die Anwendung von Mikrobüretten mit erheblichen Fehlern behaftet. Es galt folglich, eine Methode zur Feinwasserbestimmung ausfindig zu machen, welche die genannten Fehlerquellen ganz oder zumindest teilweise vermeidet. In the case of very low water contents, the Fischer method is unavoidable introduction of small amounts of water from the humid room air the need to dilute the Fischer solution and through the use of microburettes fraught with significant errors. It was therefore a matter of finding a method for determining fine water to find out which of the sources of error mentioned are wholly or at least partially avoids.

Erfindungsgemäß können Feinwasserbestimmungen auf coulometrischem Wege unter Anwendung einer modifizierten Fischer-Lösung vorgenommen werden. According to the invention, fine water determinations can be based on coulometric Ways can be made using a modified Fischer solution.

Die modifizierte Fischer-Lösung zeichnet sich dadurch aus, daß das für die Wasserbestimmung erforderliche Jod nicht wie bisher in freier, sondern in latenter Form - als geeignetes Alkyljodid - enthalten ist. Bei der Elektrolyse von Alkyljodiden in einer ansonsten jodfreien Fischer-Lösung wird anodisch Jod gebildet, welches in bekannter Weise nach der von Karl Fischer angegebenen Reaktion mit vorhandenem Wasser reagiert. Diese Reaktion verläuft in unmittelbarer Umgebung der Anode so rasch, daß auch bei starkem Durchmischen der Lösung keine unerwünschte Sekundärreaktion durch kathodisch gebildeten Wasserstoff, also auch keine Reduktion einmal frei gemachten Jods zu Jodwasserstoff, erfolgt. Apparativ elegant wird das Verfahren, wenn das für die Elektrolyse erforderliche Elektrodenpaar zugleich als Vibrationsrührer ausgebildet ist.The modified Fischer solution is characterized by the fact that the The iodine required for water determination is not, as before, in free, but in latent form - as a suitable alkyl iodide - is included. In the electrolysis of Alkyl iodides in an otherwise iodine-free Fischer solution, iodine is formed anodically, which in a known manner according to the reaction given by Karl Fischer with existing Water reacts. This reaction takes place in the immediate vicinity of the anode quickly that, even with vigorous mixing of the solution, no undesired secondary reaction by cathodically formed hydrogen, i.e. no reduction once released Iodine to hydrogen iodide. The process becomes elegant in terms of apparatus if that The pair of electrodes required for electrolysis is also designed as a vibration stirrer is.

Die Endpunktanzeige kann in bekannter Weise nach der Dead-stop-Methode erfolgen, wobei sich zugleich einfache Möglichkeiten einerAutomatisierungetwa durch Unterbrechung des Elektrolysestromes bei Erreichen des Endpunktes - ergeben.The end point display can be carried out in a known manner using the dead-stop method take place, at the same time simple possibilities of automation, for example Interruption of the electrolysis current when reaching the end point - result.

Die analytische Auswertung erfolgt nach den Grundsätzen der Coulometrie, wie überhaupt die Messung der zum Erreichen des Endpunktes erforderlichen Strommenge mit einem Coulometer üblicher Art vorgenommen wird. The analytical evaluation is carried out according to the principles of coulometry, as well as the measurement of the amount of electricity required to reach the end point is carried out with a conventional type of coulometer.

PATENTANSPROCHE: 1. Verfahren zur coulometrischen Wasserbestimmung nach einer modifizierten Karl-Fischer-Methode, dadurch gekennzeichnet, daß die Fischer-Lösung latentes Jod in Form eines geeigneten Alkyljodides (z. B. Methyljodid) enthält, welches bei Elektrolyse das für die Fischer-Reaktion zur Wasserbestimmung erforderliche Jod liefert. PATENT CLAIM: 1. Method for coulometric water determination according to a modified Karl Fischer method, characterized in that the Fischer solution contains latent iodine in the form of a suitable alkyl iodide (e.g. methyl iodide), which, in the case of electrolysis, is the one required for the Fischer reaction to determine water Iodine supplies.

Claims (1)

2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Elektrolyseelektroden zugleich als Vibrationsrührer ausgebildet werden und ein getrenntes Paar von Indikatorelektroden zur Deadstop-Endpunktanzeige benutzt wird. 2. The method according to claim 1, characterized in that the electrolysis electrodes at the same time be designed as a vibration stirrer and a separate pair of indicator electrodes is used to indicate the dead stop end point. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die analytische Auswertung nach der Aquivalenz von geflossener Strommenge und erzeugtem Jod bzw. gebundenem Wasser erfolgt. 3. The method according to claim 1, characterized in that the analytical Evaluation according to the equivalence of the amount of electricity flowed and the iodine generated or bound water takes place.
DEO6157A 1958-05-09 1958-05-09 Method for coulometric water determination Pending DE1086918B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEO6157A DE1086918B (en) 1958-05-09 1958-05-09 Method for coulometric water determination

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEO6157A DE1086918B (en) 1958-05-09 1958-05-09 Method for coulometric water determination

Publications (1)

Publication Number Publication Date
DE1086918B true DE1086918B (en) 1960-08-11

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Family Applications (1)

Application Number Title Priority Date Filing Date
DEO6157A Pending DE1086918B (en) 1958-05-09 1958-05-09 Method for coulometric water determination

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Country Link
DE (1) DE1086918B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0127740A1 (en) * 1980-10-20 1984-12-12 Riedel-De Haen Aktiengesellschaft Titration reagent for the determination of small amounts of water and method of using it
WO1984004968A1 (en) * 1983-06-10 1984-12-20 Tno Process of determination of the concentration of halogen in organic samples

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0127740A1 (en) * 1980-10-20 1984-12-12 Riedel-De Haen Aktiengesellschaft Titration reagent for the determination of small amounts of water and method of using it
WO1984004968A1 (en) * 1983-06-10 1984-12-20 Tno Process of determination of the concentration of halogen in organic samples
US4778570A (en) * 1983-06-10 1988-10-18 Nederlandse Centrale Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Process for determining the organic halogen content of organic samples

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