Gpc sec software

Molecular weights
and dispersities were determined for the various homopolymers and
diblock copolymers using an Agilent 1260 Infinity GPC instrument.
The setup comprised a pump, a degasser, three columns in series (PL-Aquagel
Mixed-H, OH-30, and OH-40), and a refractive index detector. The column
and detector temperature was set at 30 °C, and the flow rate
was 1.0 mL min^–1. Calibration was achieved using
nine near-monodisperse poly(ethylene oxide) standards (2.1–969
kDa), and data were analyzed using Agilent Technologies GPC/SEC software.
For PMPC_x and its copolymers, the eluent
was an aqueous solution containing 0.20 M NaNO₃ and 0.05
M Trizma buffer at pH 7.0. For PATAC_x and
its copolymers, the eluent was an aqueous solution containing 0.50
M CH₃COOH and 0.30 M NaH₂PO₄ at pH
2.0. For PAMPS_x and its copolymers, the
eluent was a 70% v/v aqueous solution containing 0.20 M NaNO₃ and 0.01 M NaH₂PO₄ at pH 7.0, with 30% v/v
methanol.

An Agilent Infinity II MDS instrument equipped with differential refractive index (DRI), viscometry (VS), dual-angle light scatter (LS) and variable wavelength UV detectors (set at 309 nm) was used for all SEC analysis. The system was fitted with 2× PLgel Mixed D columns (300 × 7.5 mm) and a PLgel 5 μm guard column. The eluent utilized was DMF with 5 mmol NH₄BF₄ additive at a flow rate of 1.0 mL·min⁻¹ at 50°C. Poly(methyl methacrylate) standards (Agilent EasyVials) were used for calibration between 955 000 and 550 g·mol⁻¹. Samples were prepared in the mobile phase and passed through a nylon membrane with 0.22 μm pore size prior to injection. Agilent GPC/SEC Software was used to determine experimental molar mass (M_nSEC), experimental molecular weight (M_wSEC) and dispersity (Đ) of synthesized polymers.

Size exclusion chromatography
(SEC) analysis
was performed on two systems: DMF-SEC: Agilent 390-LC MDS instrument
equipped with differential refractive index, viscometry, dual angle
light scatter, and dual wavelength UV detectors. The system was equipped
with 2 × PLgel Mixed D columns (300 × 7.5 mm) and a PLgel
5 μm guard column. The eluent is DMF with 5 mmol NH₄BF₄ additive. Samples were run at 1 mL min^–1 at 50 °C. Poly(methyl methacrylate) standards (Agilent EasyVials)
were used for calibration, MW ranging from 550 to 2.14 × 10⁶ g mol^–1. Analyte samples were filtered
through a nylon membrane with 0.22 μm pore size before injection.
Experimental molar mass (M_n,_SEC) and dispersity (D̵) values of synthesized polymers were determined
by conventional calibration using Agilent GPC/SEC software.
Dimethylacetamide (DMAC)-SEC was performed on a Shimadzu modular
system comprising an SIL-20AD automatic injector, a RID-10A differential
refractive-index detector, and a 50 × 7.8 mm guard column followed
by three KF-805L columns (300 × 8 mm, bead size: 10 μm,
pore size maximum: 5000 Å). N,N-dimethylacetamide (DMAc, 0.03% LiBr) was used as the eluent with
a flow rate of 1 mL min^–1 at 50 °C. Samples
were filtered through 0.45 μm poly(tetrafluoroethylene) filters
before injection. The SEC calibration was performed with polystyrene
standards, ranging from 500 to 2 × 10⁶ g mol^–1.

¹H (600 MHz) and ¹³C NMR (150 MHz) spectra were recorded on a Varian NMR 600 MHz spectrometer at room temperature, using the residual protic solvent signal in the deuterated solvent for calibration (chloroform-d at δ 7.26 ppm). Chemical shifts are reported in ppm. Spin multiplicities are reported as a singlet (s), doublet (d), triplet (t) or multiplet (m) with coupling constants (J) given in Hz, where applicable. Tensile stress–strain experiments were carried out using an AML X5-500 single column universal tester, equipped with a 5 kN load cell and wedge grips. Specimens with dimensions of 40 mm × 5.0 mm × c. 0.3 mm were cut from the films for testing. The samples were analysed at a strain rate of 100 mm min⁻¹. The instrument was calibrated according to the requirements of ISO 7500-1. Size exclusion chromatography (SEC) was conducted using a Polymer Laboratories PL-GPC 220 high temperature chromatograph equipped with PL Mixed Gel columns at 40 °C eluting with analytical grade chloroform. Samples were dissolved in the same solvent (at 5 mg mL⁻¹ concentration) and filtered through a syringe filter (0.2 µm) prior to injection. Molecular weight data were processed using standard Agilent GPC/SEC software and are reported in comparison to ‘PL Easy-Cal’ polystyrene standards.

Size exclusion chromatography (SEC) analysis was performed on an Agilent Infinity II MDS instrument equipped with differential refractive index (DRI), viscometry (VS), dual angle light scatter (LS) and variable wavelength UV detectors. The system was equipped with 2× PLgel Mixed D columns (300 × 7.5 mm) and a PLgel 5 μm guard column. The mobile phase used was DMF (HPLC grade) containing 5 mM NH₄BF₄ at 50 °C at flow rate of 1.0 ml min⁻¹. Poly(methyl methacrylate) (PMMA) standards (Agilent EasyVials) were used for calibration between 955 000–550 g moL⁻¹. Analyte samples were filtered through a nylon membrane with 0.22 μm pore size before injection. Number average molecular weights (M_n), weight average molecular weights (M_w) and dispersities (Đ_M = M_w/M_n) were determined by conventional calibration and universal calibration using Agilent GPC/SEC software.

DMF gel permeation
chromatography (GPC) was used to assess the molecular weight distribution
of each (co)polymer. The instrument setup comprised two Agilent PL
gel 5 μm Mixed-C columns and a guard column connected in series
to an Agilent 1260 Infinity GPC system operating at 60 °C. The
GPC eluent was high-performance liquid chromatography-grade DMF containing
10 mM LiBr at a flow rate of 1.0 mL min^–1, the copolymer
concentration was typically 1.0% w/w, and calibration was achieved
using a series of ten near-monodisperse poly(methyl methacrylate)
(PMMA) standards ranging from 1080 to 905,000 g mol^–1. Chromatograms were analyzed using Agilent GPC/SEC software.

An Agilent 1260
Infinity GPC system equipped with a differential refractive index
detector and a UV detector was used to determine the number-average
molecular weight (M_n), weight-average
molecular weight (M_w), and dispersity
(M_w/M_n) for
each (co)polymer. Two Agilent PL-gel 5 μm mixed-C columns and
a guard column were connected in series to this GPC system. Unless
otherwise stated, high-performance liquid chromatography (HPLC) grade
DMF containing 10 mM LiBr was used as the eluent. GPC analysis was
performed at 60 °C using a constant flow rate of 1.0 mL min^–1. A series of near-monodisperse poly(methyl methacrylate)
calibration standards with M_p values ranging
from 800 g mol^–1 to 2 200 000 g mol^–1 were used to calculate molecular weights and dispersities.
All (co)polymer samples were diluted to 1.0% w/w using the GPC eluent
and chromatograms were analyzed using Agilent GPC/SEC software.