Sample Name: Poly(styrene-b-ethylene oxide) 1H NMR spectrum of the sample Sample #: P3207-SEO p3207-SEO 3.65 ppm Structure: CH2 CH b n CH2 CH2 O m 6.4 7.2 ppm Composition: Mn x 103 S-b-EO 51.0-11.5 PDI 1.05 2.36 1.0 Synthesis Procedure: Poly(styrene-b-ethylene oxide) diblock copolymer is prepared by living anionic polymerization. SEC profile of the block copolymer P3207-SEO Characterization: The molecular weight and polydispersity index (PDI) of the block copolymer are characterized by size exclusion chromatography (SEC). The composition of the block copolymer was calculated from 1H-NMR by comparing the peak area of the phenyl polystyrene protons between 6.4 to 7.2 ppm and the ethylene oxide protons at 3.65 ppm. Solubility: The polymer is soluble in THF (at 35 °C), CHCl3, benzene, toluene, dioxane. Low molecular weight SEO with high contents of the polyethylene oxide block can also be solubilized in methanol and water. 18 19 20 21 22 23 24 25 26 27 28 29 Ve (ml) Size exclusion chromatography of poly(styrene-b-ethylene oxide) Poly(styrene), Mn=51000, Mw=53500, PI=1.05 Block Copolymer PSt(51000)-b-PEO(11500), PI=1.05 Composition from H NMR Thermal analysis of the sample# P3207-SEO Thermal analysis results at a glance Thermal analysis of the samples was carried out on a TA Q100 differential scanning calorimeter at a heating rate of 20oC/min.The midpoint of the slope change of the heat flow plot of the second heating scan was considered as the glass transition temperature (Tg). For PS block Tg: 86oC For PEO block Tg: -61oC Tm: 53oC Tc: -32oC Thermogram for the sample Melting and crystallization curve for the PEO block For PEO block: The melting temperature (Tm) was taken as the maximum of the endothermic peak where as the crystallization temperature (Tc) was considered as the minimum of the exothermic peak. -0.2 -0.3 -72.57°C -0.4 -60.96°C(T) -0.6 -55.72°C -0.5 Heat Flow (W/g) Heat Flow (W/g) -0.4 -0.6 -0.8 -1.0 -0.7 -80 -75 -70 -65 -60 Exo Up -55 -50 -45 -40 53.12°C -1.2 Universal V4.2E TA Instruments Temperature (°C) For PS block -1.4 20 30 40 50 Exo Up 60 70 80 Universal V4.2E TA Instruments Temperature (°C) 0.70 0.8 -31.61°C 0.65 0.6 0.60 Heat Flow (W/g) Heat Flow (W/g) 90.60°C 85.71°C(T) 72.72°C 0.55 0.4 0.50 50 Exo Up 60 70 80 Temperature (°C) 90 100 Universal V4.2E TA Instruments 0.2 -45 Exo Up -40 -35 -30 Temperature (°C) -25 -20 Universal V4.2E TA Instruments
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