400 mhz dmx instrument

HSQC NMR experiments
were performed
for the structural characterization and semi-quantification of hemicelluloses
and lignin in the extracts. A Bruker 400 MHz DMX instrument (Bruker
Corporation, Billerica, MA, USA) equipped with a multinuclear inverse
Z-grad probe was used. The pulse sequence was hsqcetgpsi. The pulse
length was optimized at 9.2 s with a 1.49 s relaxation delay and 176
scans per sample. For each experiment, approximately 70 mg of sample
was dissolved in 550 μL of DMSO-d₆. Phase correction in the spectra was performed manually, and baseline
correction was performed using a third-order Bernstein polynomial
fit. Peak assignment was made according to previous work.^{11 (link),23 (link),24 (link)} Calculations on the quantification
of interunit linkages are provided as Supporting Information.
³¹P NMR experiments were conducted
according to previous work,^{25 (link)} following
the protocol by Argyropoulos.^{26 (link)} Peak assignments
were made according to the study by Pu et al.^{27 (link)} A Bruker Avance III HD 400 MHz instrument with a BBFO probe equipped
with a Z-gradient coil was used. The pulse sequence zgig30 was used,
with 256 scans and a relaxation delay (D1) of 6 s. The spectra were
processed with MestreNova (Mestrelab Research).

HSQC NMR experiments
were performed
for the structural characterization and semi-quantification of hemicelluloses
and lignin in the extracts. A Bruker 400 MHz DMX instrument (Bruker
Corporation, Billerica, MA, USA) equipped with a multinuclear inverse
Z-grad probe was used. The pulse sequence was hsqcetgpsi. The pulse
length was optimized at 9.2 s with a 1.49 s relaxation delay and 176
scans per sample. For each experiment, approximately 70 mg of sample
was dissolved in 550 μL of DMSO-d₆. Phase correction in the spectra was performed manually, and baseline
correction was performed using a third-order Bernstein polynomial
fit. Peak assignment was made according to previous work.^{11 (link),23 (link),24 (link)} Calculations on the quantification
of interunit linkages are provided as Supporting Information.
³¹P NMR experiments were conducted
according to previous work,^{25 (link)} following
the protocol by Argyropoulos.^{26 (link)} Peak assignments
were made according to the study by Pu et al.^{27 (link)} A Bruker Avance III HD 400 MHz instrument with a BBFO probe equipped
with a Z-gradient coil was used. The pulse sequence zgig30 was used,
with 256 scans and a relaxation delay (D1) of 6 s. The spectra were
processed with MestreNova (Mestrelab Research).

Gel permeation chromatograph (GPC, Waters 1515 system, Waters Corp., Milford, MA, USA) was used to measure the dispersities (M_w/M_ns) of T_xS₄₈O₄₆S₄₈T_x pentablock terpolymers with polystyrene as the calibration standard and THF as the eluent (1.0 mL/min) at 40 °C. Number-average molecular weights (M_ns) of T_xS₄₈O₄₆S₄₈T_x and A_xS₄₈O₄₆S₄₈A_x were determined from their ¹H NMR spectra, which were recorded on a Bruker DMX-400 MHz instrument (Bruker Corp., Karlsruhe, Germany).
Dynamic light scattering (DLS) measurements of A_xS₄₈O₄₆S₄₈A_x micelle solutions were performed on a Brookhaven BI-200SM Instrument (Brookhaven Instruments Corp., Holtsville, NY, USA). with a laser wavelength of 657 nm at 25 °C. The scattering angle was fixed at 90°. The Zeta potentials ξ of A_xS₄₈O₄₆S₄₈A_x micelles were also measured by electrophoretic light scattering (ELS) using the same BI-200SM Instrument.
The morphologies of A_xS₄₈O₄₆S₄₈A_x micelles were observed by cryogenic transmission electron microscopy (cryo-TEM) on a Talos F200C cryogenic electron microscopy (FEI Company, Hillsboro, Oregon) at an acceleration voltage of 200 kV. The micelle solutions were dropped onto bare copper grids, which were immediately submerged into liquid nitrogen for flash freezing. The cryo-grids were then mounted on a cryogenic sample holder. Images were recorded on a Ceta 4 K × 4 K camera with a resolution ratio ≤0.3 nm.