Biospin av 300 spectrometer

NMR spectra were recorded using a Bruker (MA, USA) BioSpin AV-300 spectrometer. Gel permeation chromatography (GPC) measurements were conducted using a system consisting of a JASCO (Tokyo, Japan) PU-2089 pump, a JASCO CO-2065 column oven, a JASCO RI-2031 refractive index detector, and a Shodex OHpak SB-804 HQ column (8.0 × 300 mm, SHOWA DENKO, Tokyo, Japan). A phosphate buffer (20 mM, pH 7.0) containing 20% N,N-dimethylformamide was used as the eluent at a flow rate of 0.5 mL/min at 30 °C. Pullulan samples were used as standards. Transmittance was recorded using a Hitachi (Tokyo, Japan) U-2000 spectrometer. Dynamic light scattering (DLS) analyses were conducted using an Otsuka Electronics (Osaka, Japan) ELSZ-1000 at 667 nm. The samples for transmittance and DLS analyses were prepared using 0.5 wt % in aqueous media and filtered through a membrane filter (0.45 μm). The fluorescence intensity was recorded using a JASCO FP-6500 spectrometer.

The ¹H NMR spectra were recorded using a ECX400 (JEOL, Akishima, Tokyo, Japan), ECA600 (JEOL), and a BioSpin AV-300 spectrometer (Bruker, Yokohama, Kanagawa, Japan). The powder XRD measurements were performed using a X’Pert Pro MPD diffractometer (PANalytical B.V., Almelo, The Netherlands) with Ni-filtered Cu Kα radiation (λ = 0.15418 nm). GPC measurements were conducted using a system consisting of a LC-20AD pump (Shimadzu, Kyoto, Japan), a CTO-10A column oven, an RID-10A refractive index detector, and two TSK gel Super HZM-N (4.6 × 150 mm; TOSOH, Tokyo, Japan) columns. Chloroform was used as the eluent at a flow rate of 0.25 mL/min at 40 °C. Polystyrene samples were used as standards. The DMA were performed using a DMA 2980 Dynamic Mechanical Analyzer (TA Instruments, Tokyo, Japan) at heating rate of 5 °C/min at 1 Hz using a supramolecular polymeric film (5 mm × 20 mm).