The 13C cross polarization (CP) magic angle spinning (MAS) Nuclear magnetic resonance spectroscopy (NMR) measurements were performed using an Agilent DD2 600 spectrometer (Agilent Technologies, USA), with magnetic flux density of 14.1 T and equipped with a 3.2 mm T3 MAS NMR probe operating in double resonance mode. The MAS rate in experiments was 10 kHz, the number of scans was 10 000 with a 6.0 s delay between successive scans, and CP contact time was 1.3 ms. The spectra were processed using TopSpin 3.5 and OriginPro 2017 software. Deconvolution of the peak was carried out using OriginPro 2017 software (Multiple Peak Fit) and Gaussian functions. Deconvolution was performed based on the studies of Duer et al.34 (link) and Idris et al.12 (link)
3.2 mm t3 mas nmr probe
Manufactured by Agilent Technologies
Sourced in United States
The 3.2 mm T3 MAS NMR probe is a laboratory equipment designed for use in Nuclear Magnetic Resonance (NMR) spectroscopy. It features a 3.2 mm sample coil diameter and is capable of magic-angle spinning (MAS) for solid-state NMR analysis.
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2 protocols using 3.2 mm t3 mas nmr probe
1
Solid-State NMR Spectroscopy of Materials
2
Evaluating Wood Delignification and Dissolution
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Wood
delignification and IL-facilitated partial dissolution were verified
with a Thermo Scientific Nicolet iS50 FTIR spectrometer with an attenuated
total reflectance (ATR) diamond (Thermo Scientific, USA). All spectra
were collected in the absorption mode in the 400–4000 cm–1 wavelength range from 32 scans with a resolution
of 4 cm–1. The 13C cross polarization
(CP) magic angle spinning (MAS) NMR measurements were performed using
an Agilent DD2 600 NMR spectrometer with a magnetic flux density of
14.1 T, equipped with a 3.2 mm T3 MAS NMR probe operating in a double-resonance
mode. Samples were packed in ZrO2 rotors, and the MAS rate
in experiments was set to 10 kHz. A total of 14,000 scans were accumulated
using a 1.3 ms contact time and a 5.0 s delay between successive scans.
Protons were decoupled during acquisition using SPINAL-64 proton decoupling
with a field strength of 80 kHz. 90° pulse durations and Hartmann–Hahn
match for CP were calibrated using a-glycine. The spectra were processed
using TopSpin 3.5 software. The changes in the crystallinity of the
wood after delignification and partial dissolution with the IL were
estimated from signal areas of the cellulose C4 carbon
signals originating from crystalline (89.0–84.4 ppm) and noncrystalline
(84.4–77.3 ppm) regions. Signal areas were determined by integration.
delignification and IL-facilitated partial dissolution were verified
with a Thermo Scientific Nicolet iS50 FTIR spectrometer with an attenuated
total reflectance (ATR) diamond (Thermo Scientific, USA). All spectra
were collected in the absorption mode in the 400–4000 cm–1 wavelength range from 32 scans with a resolution
of 4 cm–1. The 13C cross polarization
(CP) magic angle spinning (MAS) NMR measurements were performed using
an Agilent DD2 600 NMR spectrometer with a magnetic flux density of
14.1 T, equipped with a 3.2 mm T3 MAS NMR probe operating in a double-resonance
mode. Samples were packed in ZrO2 rotors, and the MAS rate
in experiments was set to 10 kHz. A total of 14,000 scans were accumulated
using a 1.3 ms contact time and a 5.0 s delay between successive scans.
Protons were decoupled during acquisition using SPINAL-64 proton decoupling
with a field strength of 80 kHz. 90° pulse durations and Hartmann–Hahn
match for CP were calibrated using a-glycine. The spectra were processed
using TopSpin 3.5 software. The changes in the crystallinity of the
wood after delignification and partial dissolution with the IL were
estimated from signal areas of the cellulose C4 carbon
signals originating from crystalline (89.0–84.4 ppm) and noncrystalline
(84.4–77.3 ppm) regions. Signal areas were determined by integration.
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