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Polymers 2021, 13, 1386 3 of 14 Polymers 2021, 13, x FOR PEER REVIEW 4 of 15 (2) 20 -10 ppm 10 0 ppm-10 (a) 1H PFG -NMR water 10 0 (b) 1H PFG -NMR for the bare sulfonated polysulfone (SPSf), composite silica-SPSf (SPSf-SiO2) and composite acidic silica-SPSf (SPSf-SiO2_sulf), respectively. NMR measurements were performed with a Bruker NMR spectrometer AVANCE 300 Wide Bore working at 300 MHz on 1H (Bruker, Milan, Italy), equipped with multinuclear Diff30 Z-diffusion probe for pulse field gradient (PFG) measurements. Self-diffusion coeffi- cients of water and methanol were performed by using the pulsed field gradient spin−echo (PFGSE) method [41]: the sequence consists of three 90◦ rf pulses (π/2-τ1-π/2-τm-π/2) and two gradient pulses that are applied after the first and the third rf pulses, respectively. The echo is found at time τ = 2τ1 + τm. For illustrative purposes, the 1H PFG NMR spectra corresponding to water and methanol absorbed in sPSf filler-free are shown as a function of the amplitude of the field gradient in Figure 1a,b, respectively. Following the usual nota- tion, the magnetic field gradient pulses have magnitude g, duration δ, and time delay ∆. The FT echo decays were analyzed by means of the relevant Stejskal–Tanner expression: I = I0e−KD (1) where, I and I0 represent the intensity/area of a selected resonance peak in the presence and in absence of gradients, respectively. K is the field gradient parameter, defined as: 1 0.1 0.01 water (c) sPSF filler-free sPSF/SiO2 sPSF/SiO2-sulf 0 1×1010 Κ (s m-2) 3×1010 1◦ Figure 1. H PFG NMR spectra corresponding to (a) water and (b) methanol absorbed in the Pebax membrane at 20 C. Figure 1. 1H PFG NMR spectra corresponding to (a) water and (b) methanol absorbed in the Pebax membrane at 20 °C. (c) 22 (cP)lPotlootfotfhtehenonromrmalaizliezdedpepaekakaraeraesavssv.sK. K((γ((gγδg)δ)(Δ(-∆δ−/3δ))/f3o)r) fwoartweracteorncfionnefidniendtihnettherethermeembemrabnreasn. Tesh.eTshoelisdolgirdeegnreleine represents the linear fitting to the experimental data. line represents the linear fitting to the experimental data. IInnththeesseeeexxppeerriimeenttss,, δδaannd∆Δweerreekkeeppttaatt00.8.8mssaanndd88mss, ,rreessppeecctitviveelyly, ,ththeeeecchhoo K= (γgδ)2(∆− 3δ)] 2×1010 methanol M/M0 titmimeewaass55.7.7mss,,whhilieleggwaassvvaarireieddbbeetwtweenen10100anandd80800GGcmcm ,incrementtediin12sttepss.. The number of scans for the 1H PFG-NMR measurements were 4, while the number of repetitions was kept equal to 2. The repetition time was about 5 times the longitudinal relaxation time (T1) and the total acquisition time ranged between 2 and 10 min. Figure 1c illustrates the experimental echo-signal attenuation curves in the diffusion measurements for water and methanol in the three membranes. On the basis of the very high SNR (signal to noise ratio), the attenuation higher than 90%, the low standard deviation of the fitting −1 −1PDF Image | Properties of Methanol Transport for Direct Methanol Fuel Cells
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