Analytical Sciences

Abstract − Analytical Sciences, 30(7), 767 (2014).

Decomposition Procedure Using Methyl Orthoformate to Analyze Silicone Polymers
Yuichiro FUJIMOTO,* Keisuke SOGABE,* and Hajime OHTANI**
*Kaneka Techno Research Corporation, 5-1-1 Torikainishi, Settsu, Osaka 566-0072, Japan
**Department of Materials Science and Engineering, Graduate School of Engineering, Nagoya Institute of Technology, Gokiso, Showa, Nagoya, Aichi 466-8555, Japan
A new decomposition method for structural analysis of polysiloxanes (silicones) was developed using methyl orthoformate. The siloxane bonds in samples with vinyl and/or methyl side groups decomposed under relatively mild acidic conditions up to around 70°C and were followed by methoxylation at the cleaved linkages with few side reactions. The product yields with respect to the siloxane monomer units were 98 – 100% for low molecular weight model siloxane compounds. Additionally, this method decomposed the silicone polymer sample in a similar manner with decomposition yields of 98 and 103% for the dimethylsiloxane main chain and dimethylvinylsilyl end groups, respectively. These results demonstrate that the proposed decomposition method should be an effective pretreatment procedure for structural and compositional analyses of silicone polymers.