Evaluation of hydrogen dissolved in rubber materials under high-pressure exposure using nuclear magnetic resonance

Hydrogen molecules dissolved in rubber due to high-pressure hydrogen gas exposure have been analyzed using 1H nuclear magnetic resonance (NMR) with solution and solid-state probes. To analyze the characteristics of dissolved hydrogen in rubber materials and to compare them with gaseous phase hydrogen, we measured the NMR spectra of gaseous phase hydrogen and evaluated the chemical shifts and pressure dependency. Measurement using a sealed tube and liquid phase probes enabled the simultaneous analysis of dissolved hydrogen in rubber and gaseous phase hydrogen eliminated from the rubber. Two peaks at 4.3 and 4.8 p.p.m. were observed in the 1H MAS NMR of the rubber samples after high-pressure hydrogen exposure. Using information from the chemical shift of the free hydrogen gas and the time dependency of hydrogen quantification in the rubber, both of these peaks were confirmed to be attributable to dissolved hydrogen. Their differences in relaxation time confirmed that their mobilities were different. In conclusion, the hydrogen dissolved in acrylonitrile butadiene rubber exists in two different forms with different mobilities. The ratio of those two hydrogens differs and is affected by the exposure pressure and elimination process time. Polymer Journal (2012) 44, 832–837; doi:10.1038/pj.2012.111; published online 27 June 2012