The 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 per molecule.