Sample Name: Poly(N-isopropyl acrylamide) Sample #: P5542-NIPAM Structure: CH2 CH C n O NH CH H3C CH3 Composition: Mw x 103 Mn x 103 PDI 1,800.0 1,400.0 1.3 Solution Viscosity : [η]= in CH3OH at 25 oC: Purification of polymer: Unreacted monomer was removed by dissolving the product in cold water than warming the solution. The polymer separated out. This procedure was applied 2 times to remove the unreacted monomer. The obtained polymer was dissolved in acetone and reprecipitated in cold ether. Solubility: Poly(N-isopropyl acrylamide) is soluble in water, DMF, THF, acetone, insoluble in hexane and ether. SEC of Homopolymer: P5542-NIPAM 2.64dl/g Viscotek Triple Detector Concentration (RI) Light Scattering Viscosit Synthesis Procedure: Poly(N-isopropyl acrylamide) is obtained by free radical process Characterization: The molecular weight and polydispersity index (PDI) were obtained by size exclusion chromatography (SEC) in THF. SEC analysis was performed on a Varian liquid chromatograph equipped with refractive and UV light scattering detectors. Three SEC columns from Supelco (G6000-4000-2000 HXL) were used with triple detectors from Viscotek Co. Sample Preparation: Polymer sample for the GPC were prepared as reported in the literature (Macromolecules, 2000,33,6738). To avoid the effect of concentration and the amount of water present in the sample, on line triple detectors were used and the dn /dc was calculated and found : 0.034mL/g in THF at 35 oC. In this case the polymer was not eluted in our columns used in SEC. DMF was found good solvent to elute such high molecular polymer polymer. Mw/Mn was therefore determined by eluting the polymer in DMF. The solution viscosity was determined in methanol: Viscosity measurement was carried out in a Ubbelohde viscometer at 25°C. Four solutions in methanol of different concentrations were measured. The intrinsic viscosity was obtained by extrapolation to c=0. From viscosity-molecular weight relationship [η]= 2.9910-2 M0.64 (Makromolecular Chem. V180, P969, 1979), the viscosity average molecular weight was calculated accordingly. 10 15 20 25 Ve RI (mV) 0 0 2 4 6 8 10 Ve (ml) Size Exclusion Chromatography of Poly N-isopropylacrylamide(NIPAM) Carried out in DMF at 40 oC. Mn = 1,400,000, Mw = 1800,000, Mw/Mn = 1.3
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