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Separation of 13C spectra of polyurethane soft and hard segments by ROSY_NM200013E

Separation of 13C spectra of polyurethane soft and hard segments by ROSY

The ROSY (Relaxation Ordered SpectroscopY) is a method in which the 13C CPMAS spectrum of a mixture is classified by a longitudinal relaxation time of 1H, and the 13C CPMAS spectrum is displayed separately for each substance. In solution NMR, each peak in the 1H spectrum has its own longitudinal relaxation time. In solid-state NMR, however, spin diffusion occurs due to the dipolor interaction between 1H, and all 1H have the same longitudinal relaxation in the domain within a certain distance. The 13C spectrum can be separated for each domain by using this difference in relaxation time of 1H. The longitudinal relaxation time (T1H) obtained by the saturation recovery method as shown in Fig.1a is usually used to separate the 13C spectrum of the mixture. The size of the domain that can be separated by this method is about 100 nm. To separate domains smaller than this, a measurement using the relaxation time at rotational flame (TH) obtained by the spinlock method as shown in Fig.1b is effective. The domain size that can be separated by TH is about several nm, and it is possible to determine the phase separation structure of block copolymers and the molecular compatibility.

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