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Vxr 400 mhz

Manufactured by Agilent Technologies
Sourced in United States

The VXR 400 MHz is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for advanced analytical applications. It features a 400 MHz superconducting magnet and delivers reliable, high-resolution data for a wide range of samples.

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3 protocols using vxr 400 mhz

1

Characterization of Polymer Properties

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1H NMR spectra were recorded
at room temperature on a Varian VXR 400 MHz (1H: 400 MHz)
spectrometer using deuterated solvents. Chemical shifts (δ)
are reported in ppm, whereas the chemical shifts are calibrated to
the solvent residual peaks. Gel permeation chromatography (GPC) measurements
were performed in THF at 25 °C (1 mL/min) on a Spectra-Physics
AS 1000, equipped with PLGel 5 μm × 30 cm mixed-C columns.
Universal calibration was applied using a Viscotek H502 viscometer
and a Shodex RI-71 refractive index detector. The GPC was calibrated
using narrow disperse polystyrene standards (Polymer Laboratories).
Melt rheology was carried out via a TA Instruments AR 1000 under nitrogen
flow, and 25 mm parallel plate geometries and interplate gap of 0.8–1
mm were used in all cases. Samples were vacuum-dried overnight before
use. All measurements were performed in the linear viscoelastic regime,
determined via torque sweep measurements. Frequency sweeps were carried
out at different temperatures (for PTHY100 they were 40, 45, 55, 65,
75, 85, and 90 °C), and for the reproducibility of the data the
measurement at Tr was
repeated. In all cases, the repeated frequency sweeps were the same
within 5% error.
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2

Comprehensive Physicochemical Characterization of Polyhydroxylurethanes

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FTIR (Fourier transform infrared) spectra were recorded on a Nicolet iS5 Mid Infrared FT-IR Spectrometer equipped with iD7 ATR optical base (Thermo Scientific®, Waltham, MA, USA). 1H NMR spectra were recorded on a Varian VXR 400 MHz (Palo Alto, Santa Clara, CA, USA) using tetramethyl silane as an internal standard. Samples of 85 mg were dissolved in deuterated DMSO-d6. DSC (Differential scanning calorimetry) measurements were carried out using a Q200 DSC (TA Instruments, New Castle, DE, USA). The heating rate was 10 °C min−1. The measurements were performed on 20 mg samples in closed aluminum trays in the constant flow of argon 10 mL min−1. Viscosity was measured on a Kinexus rheometer (Netzsch, Selb, Germany) with (8-mm diameter) plate–plate geometry at 140 °C and 1/min speed. Mechanical performance of the PHUs was measured on an INSTRON 5566 (Norwood, MA, USA).
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3

Preparative Organic Chemistry Protocols

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Starting materials, unless otherwise specified, were used as high grade commercial products. Solvents were of analytical grade. Reaction progress was followed by thin layer chromatography (TLC) on precoated silica gel plates (Silica Gel 60 F254, Merck, Darmstadt, Germany and then visualized with a UV254 lamplight. Melting points were measured in glass capillary tubes on a SMP-20 apparatus (Büchi Italia, Assago, MI, Italy ) and are uncorrected. 1H-NMR and 13C-NMR experiments were recorded in CDCl3, unless differently indicated, on a VXR 400 MHz instrument (Varian, Palo Alto, CA). Chemical shifts are reported in parts per million (ppm) relative to tetramethylsilane (TMS), and spin multiplicities are given as s (singlet), d (doublet), t (triplet), m (multiplet) or br (broad). Direct infusion ESI-MS spectra were recorded on a Micromass ZQ 4000 apparatus (Waters, San Diego, CA, USA). Chromatographic separations were performed on silica gel columns (Kieselgel 40, 0.040−0.063 mm; Merck) by flash chromatography. Compounds were named relying on the naming algorithm developed by CambridgeSoft Corporation (Waltham, MA, USA) and used in ChemDraw Professional 15.0 (PerkinElmer Inc., Waltham, MA, USA).
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