Bulletin of the Chemical Society of Japan · 1969 · 31 citations · 9 references
Natural SciencesChemistryAnalytical ChemistryElemental AnalysisInorganic ChemistryChemical Composition AnalysisGas ChromatographyInorganic Elemental AnalysisOrganic Elemental AnalysisVolatile Organic CompoundsChromatographic BehaviorClaisen CondensationInfrared SpectraInorganic Composition AnalysisIonic Radius EffectsRare Earth Element ChemistryRare-earth CompoundsVolatilization
Abstract The gas chromatographic behavior of Sc, Y, and rare earth chelates of a new β-diketone, pivaroyltrifluoroacetone (PTA), was investigated. PTA was synthesized by a Claisen condensation from pinacolin and ethyltrifluoroacetone. Sc, Y, Nd, Sm, Eu, Gd, Tb, Dy, Er, Yb, and Lu PTA chelates were prepared. Their elemental analyses and infrared spectra indicated that they were anhydrous tris chelates, and the TGA curves of the chelates proved their good volatile characteristics, showing approximately a 100% weight loss. Gas chromatograms of all the chelates and of mixtures of Sc, Y, and several rare earth chelates were obtained. Some relationships were observed between the retention time, the volatilization temperature, and the ionic radius of the central metal: With the decrease in the ionic radius, the retention time of the chelate decreased and the volatilization temperature became lower.
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