Application of single-pulse solid-state 1H-MAS NMR to probe the oxidation products in crosslinked polyethylene: A detailed spectral analysis procedure

Characterisation of formulated high-density poly(ethylene) by magic angle spinning nuclear magnetic resonance

“…9 While standard procedures exist to obtain liquid-state NMR data from sample dissolution 10 or sample melting directly into an NMR tube, 11 a few different methods have been considered to prepare HDPE samples suitable for MAS NMR. These include processing the HDPE into fibers 12 or into sheet subsequently rolled into the rotor, 13 melting and pressing into a compression-moulded plate, 14 utilization of a plug the size of the rotor, 15 cutting or punching out disks the size of the internal diameter of the rotor followed by stacking [16][17][18] original pellets 19,20 and by crushing. 15 In cases where the width of the pieces of polymer created voids, inert filler was also used to enhance the weight distribution across the rotor.…”

“…13,17 These previous experiments resulted in data that identified the various structural attributes such as phase composition (crystalline, amorphous, interphase, crosslinking), crystal dimensions, molecular mobility, chain branching, deformation mechanisms, optimum methods for the quantification of phases and that probed ways in which these phase structures can be manipulated under various physical conditions. 12,14–20 However, there seems to be little consensus on the effect of the sample processing preparation methods for high resolution MAS NMR or systematic comparison between those.…”