Determination and characterization of reversed-phase bonded ligands by chemical cleavage with aqueous hydrofluoric acid.
A simple and rapid method for the determination and characterization of chemically bonded ligands on reversed-phase packing materials is described. The method consists of cleavage with aqueous concentrated hydrofluoric acid and analysis of the reaction product by GC, NMR and mass spectrometry. It is confirmed from (13)C-NMR spectra that the structure of the bonded ligand is not altered by aqueous hydrofluoric acid. Several commercial reversed-phase packing materials have been analysed by mass spectrometry and because the cleavage reaction proceeds quantitatively, the alkylsilyl groups used are completely converted into the corresponding fluoride derivatives. In the proposed method the cleavage reaction is so fast that the determination takes only 15 min for the steps prior to the chromatographic and spectrometric analyses. The relative standard deviation is 3-4%.
Miyabe
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K
Central Laboratories, Kurita Water Industries Ltd., 7-1, Wakamiya, Morinosato, Atsugi 243-01, Japan.
Orita
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