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Gpcmax ve 2001

Manufactured by Agilent Technologies
Sourced in United States

The GPCmax VE 2001 is a gel permeation chromatography (GPC) system designed for molecular weight analysis of polymers. It provides accurate and reliable measurements of the molecular weight distribution of polymeric samples.

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2 protocols using gpcmax ve 2001

1

Synthesis and Characterization of Polymeric Materials

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PEtG with a 6-nitroveratryl carbonate end-cap and alkyne-PEtG were
synthesized as previously reported.16 (link) PCL
(Mn = 55 kg/mol) was supplied by Scientific
Polymer Products, PLA (Mn = 103.5 kg/mol)
was purchased from 3D Solutech, and PHB (Mn = 550 kg/mol) was purchased from Goodfellow. CH2Cl2 was distilled from CaH2 immediately before use.
THF and toluene were distilled from sodium/benzophenone and degassed
by three freeze–pump–thaw cycles before use. DMF was
obtained from a solvent purification system using aluminum oxide columns.
NMR spectra were recorded on a 600 MHz Varian INOVA 600 instrument
or with a 400 MHz Bruker AVIII HD 400 instrument. 1H NMR
spectra were referenced to residual CHCl3 (7.27 ppm). FTIR
spectra were obtained using a PerkinElmer FTIR spectrum two instrument
in attenuated total reflectance mode. SEC was performed in THF at
5 mg/mL of the polymer using a Viscotek GPCmax VE 2001 SEC instrument
equipped with an Agilent PolyPore guard column (PL1113-1500) and two
sequential Agilent PolyPore SEC columns packed with porous poly(styrene-co-divinylbenzene) particles (MW range: 200–2 000 000
g/mol; PL1113-6500) regulated at a temperature of 30 °C. Molar
masses were calculated relative to polystyrene standards with a correction
factor of 0.56 applied to the PCL samples.38 (link)
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2

Copolymer Characterization via NMR, GPC, and DSC

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Proton nuclear magnetic resonance (1H NMR) spectroscopy was conducted on a Bruker Avance II 300 MHz spectrometer (Billerica, MA, USA), using the solvent signal as an internal reference. The composition of the copolymers was calculated using the ratios of the integral values of characteristic resonances at δH 4.0 (methylene group of PCL repeat unit), 3.6 (methylene group of PEG repeat unit), 1.1 (methyl group of PPG repeat unit) and 2.8 (methine group of epoxide end-groups) ppm.
Gel permeation chromatography (GPC) was performed on a Viscotek GPCmax (VE 2001, Houston, TX, USA) system using two PLgel Mixed-C columns (Agilent) in series and operating at 40 °C. THF was used as the eluent at a flow rate of 1 mL.min−1. OmniSEC 5.12 software (Malvern Instruments, Malvern, UK) was used to determine molecular weight characteristics based upon a conventional column calibration with narrow molecular weight polystyrene standards.
Differential scanning calorimetry (DSC) was performed on a Discovery DSC (TA Instruments, New Castle, DE, USA) under a nitrogen atmosphere. The copolymers and pure PCL were heated from 25 to 100 °C, cooled to −80 °C and then heated again to 100 °C before finally being cooled to 25 °C. All heating and cooling cycles were conducted at a ramp rate of 10 °C.min−1.
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