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Synthesis, purification, storage and isotopic analysis of CT 4 on the multicurie scale
Author(s) -
Cacaoe Fulvio,
Schüller Manfred
Publication year - 1975
Publication title -
journal of labelled compounds
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.432
H-Index - 47
eISSN - 1099-1344
pISSN - 0022-2135
DOI - 10.1002/jlcr.2590110303
Subject(s) - chemistry , isotope dilution , dilution , yield (engineering) , radiochemistry , radiolysis , mass spectrometry , impurity , gas chromatography , resolution (logic) , methane , chromatography , organic chemistry , materials science , physics , artificial intelligence , aqueous solution , computer science , metallurgy , thermodynamics
Multicurie amounts of CT 4 were prepared from T 2 via a twosteps synthesis with an overall yield of ca. 75%. After purification, the radio gas chromatographic analysis of the product revealed only a 0.5% T 2 (or HT) impurity. The isotopic analysis, carried out independently by mass spectrometry and by high‐resolution gas chromatography, showed that, immediately after preparation, tritiated methane aontained over 97.8 mol% CT 4 , with only traces of particular tritiated methanes. However self radiolysis, in particular fast intermolecular H/T scrambling, caused severe storage problems. Even after dilution with a thousand‐fold exaess of CH 4 , radiation‐induced isotopic exahanges led to serious contamination of CT 4 by partially tritiated methanes. A dramatic improvement was obtained, without further dilution of CT 4 , by addition of 1 ‐ 2 mol% NH 3 , which completely suppressed radiolytic H/T scrambling. A preparative gas chromatographic technique was developed, which allows isolation of CT 4 in a state of high radiochemical and isotopic purity.