AbstractThe combination of ultrasonic vibratory beam and gas chromatography‐mass spectrometry techniques was used to produce monomers of new organo‐multi‐silicon coating materials. The reactants of these materials were exposed to high passive conditions through all the experimental phase. By the aid of a capillary column, RTX‐5MS, and an EI detector of the Finnigan‐Mat GC, a sample was analyzed on the basis of the rules of the predominant M‐1(s) ions of the main chromatographic pattern. Fragmentation analysis of the high resolution mass spectrometry patterns led to detection of three new compound structures, designated A, B, and C isomers. These isomers were identified by the differences between their retention times. The mechanistic root for each of the three isomers is fully discussed herein by a process of stepped number of cleavages p