Zusammenfassung
Nach Verbrennung der Substanz im Sauerstoffkolben wird das Fluorid potentiometrisch mit 0,02 M Lanthan(III)-lösung bei pH 5–7 titriert. Hierbei wird eine fluoridspezifische Elektrode in Verbindung mit einem pH-Meter mit Skalendehnung verwendet. Der absolute Fehler ist kleiner als ±0,3%. Störender Schwefel wird als Bariumsulfat gefällt; Filtration ist nicht erforderlich. Phosphor muß vor der Bestimmung abgetrennt werden.
Summary
A method for the potentiometric micro- and semimicro-determination of fluorine in organic compounds is described. After combustion in a Vycor oxygen-flask, the fluoride is titrated potentiometrically with 0.02 M lanthanum (III) in an aqueous solution at pH 5–7. A fluoride ion-indicating electrode is used in conjunction with an expanded-scale pH meter. Results are within the ±0.3% absolute limits considered acceptable for microchemical analysis. The interference of sulfur is eliminated by its precipitation as barium sulfate. Filtration of the precipitate is not necessary. Phosphorus interferes and must be separated prior to fluorine analysis.
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Work performed under the auspices of the U.S. Atomic Energy Commission.
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Selig, W. Potentiometric micro- and semimicro-determination of fluorine in organic compounds. Z. Anal. Chem. 249, 30–34 (1970). https://doi.org/10.1007/BF00427242
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DOI: https://doi.org/10.1007/BF00427242