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Einsatz von Hochleistungs‐Trennkapillaren in der GC.‐EIMS./GC.‐CIMS.‐Analyse: Eine Möglichkeit zur massenspektrometrischen Doppelbindungscharakterisierung in komplexen Monoalkengemischen
Author(s) -
Blum Wolfgang,
Richter Wilhelm J.
Publication year - 1974
Publication title -
helvetica chimica acta
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.74
H-Index - 82
eISSN - 1522-2675
pISSN - 0018-019X
DOI - 10.1002/hlca.19740570626
Subject(s) - chemistry , double bond , osmium tetroxide , mass spectrometry , chromatography , organic chemistry , physics , electron microscope , optics
In an attempt to determine position and substitution of double bonds in complex mixtures of straight‐chain and branched monoalkenes without actually isolating the constituents, GC.‐MS. analysis is performed after in‐batch preparation of derivatives of a judiciously chosen type. Cyclic phenylboronates (4,5‐substituted 2‐phenyl‐1,3,2‐dioxaborols) are prepared from 1,2‐diols which are, in turn, obtained from the original alkenes by treatment with osmium tetroxide. Chemical ionization mass spectrometry (CIMS.) is used in addition to conventional electron impact techniques (EIMS.) in sequential GC./CIMS.‐ and GC./EIMS.runs, yielding complementary structural information for the single components of the mixture. In order to cope with the potential severity of the separation problem, high‐efficiency glass capillary columns were employed throughout. The performance of the system used is demonstrated by a complete double bond analysis of a 35‐component mixture of monoalkenes in the C 5 to C 9 range.