Gpc system

Fourier transform infrared (FT-IR) spectrum of F-POSS and F-POSS-Acrylate copolymer were measured by a TENSOR 27 FT-IR spectrometer (Bruker, Karlsruhe, Germany) from 400 to 4000 cm⁻¹. The samples were prepared by following the KBr pellet method. ²⁹Si NMR and 1H NMR spectrum of 7F-MAP-POSS before and after copolymerization process were recorded on a 500MHz AVANCE III spectrometer (Bruker, Karlsruhe, Germany) using CDCl₃ as a solvent. A gel permeation chromatography (GPC) system (Agilent, Palo Alto, CA, USA) was calibrated with narrow molecular weight polystyrene standards. The resulting calibration curves were used to estimate the molecular weights and polydispersity (PD) of 7F-MAP-POSS-Acrylate copolymers. THF was introduced as the mobile phase at a flow rate of 1.0 mL/min. The concentrations of samples were 5.0 mg × mL⁻¹, and the injection volume was 100 μL for each analysis. The columns and detector were maintained at 40 °C. Contact angles (CA) were measured using SL200KS contact angle analyzer (KINO, Boston, MA, USA) that had a CCD camera equipped for image capture.
Scanning electron microscopy (SEM) images and energy dispersive spectrum (EDS) were taken using a JSM-6700F scanning electron microscope (JEOL, Tokyo, Japanese). The surface morphology of the films was observed after gold was sputtered onto the surfaces.

Size-exclusion chromatograms were recorded using a GPC system from Agilent Technologies with its corresponding Agilent software, dedicated to multi-detector GPC calculation. The system used two PL1113-6300 ResiPore 3 µm 300 × 7.5 mm columns with DMF as the eluent with a flow rate of 1 mL/min and toluene as flow rate marker. The detector suite comprised a PL0390-06034 capillary viscometer, and a 390-LC PL0390-0601 refractive index detector. The entire SEC-HPLC system was thermostated at 35 °C. Low dispersity PMMA standards were used for the calibration. The typical sample concentration was 10 mg/mL. The molar masses and dispersity of the polymers were measured using universal calibration.

Molecular weights of the oligomers were measured using the GPC system (Agilent Technology, Santa Clara, CA, USA) and were calculated in comparison to polystyrene standards (PSS). The molecular weights were stated as number average molecular weight (M_n), weight average molecular weight (M_w), and dispersity value (Ð) [8 (link)].