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Karl Fischer Titration: Determination of Water by Eugen Scholz

By Eugen Scholz

The Karl Fischer titration is utilized in many various methods following its book in 1935 and extra purposes are consistently being explored. today we're experiencing one other section of growth, as proven through the advance of latest titration gear and new reagents. KF gear more and more accommodates microprocessors which allow the process a titration to be programmed therefore sim­ plifying the titration. Coulometric titrators permit water determinations within the micro­ gram-range: the KF titration has turn into a micro-method. the recent pyridine-free re­ brokers make its software considerably extra friendly and open up additional possibili­ ties because of their accuracy. To make the method of Karl Fischer titrations more uncomplicated, we have now summarized the current wisdom during this monograph and we've complemented it with our personal reports and functional adventure. As this publication may still stay "readable", we now have attempted to maintain the basics to a minimal. ancient advancements are just pointed out in the event that they appear to be valuable for figuring out the KF response. The ap­ plications are defined extra absolutely. particular information that can curiosity a selected reader are available within the unique guides stated. The referenced literature is in chronological order because the yr of ebook can also turn out informative. hence, [6902] for instance denotes sixty nine for 1969 being the 12 months of e-book and 02 is a non-recurring revolutionary quantity. The referenced litera­ ture contains summaries which we are hoping might be of support to discover the "right" publica­ tion easily.

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Example text

P. 92]. The values are not reproducible. Eberius [Eb. p. 33] compared seven KF reagents from different manufactures (Fig. 4-1, curves A-F). He found very differing loss rates. 07 mg H 20 per day (as means over a period of 20 days). "Noticeable is the titre stability of solution F, prepared by just happening to use a pyridine of unknown but effective stabilizing constituents" [Eb. p. 34]. We found a titre loss of 35% in 9 weeks for a methanolic one-component reagent using diethanolamine as a base [8002].

P. 7 mol) and 61 methanol are added. This solution can be stored indefinitely. When required, 31 of this are filled into the supply vessel of the burette and cooled with ice. 135 ml sulphur dioxide are condensed in a dry-ice/methanol cold trap and kept cold. The liquid sulphur dioxide is added to the methanol solution in the supply vessel and shaken. After cooling to room temperature, the solution is ready for use. The solution has a WE of approximately 5 mg H 20/ ml. 4 Preparation of Solutions 39 Preparation according to Eberius [Eb.

Reagents low in methanol Pyridine Methanol Sulphur dioxide Iodine Wernimont and Hopkinson Mitchell and Smith [4301] [Aqu. p. 7 g Dimethylformamide is also used as a solvent for KF reagents. 2). Sherman [8006] found the titre of the solutions to depend on the solvent which is used as the working medium. Mitsubishi applied for patents using alkyl carbonates as the solvent [8005]. 4 mol 617 ml One notable advantage of these solutions is the stability which is referenced as 10% titre loss in 300 days.

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