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56 protocols using avance 3 400 mhz nmr spectrometer

1

Purification and Characterization of Compounds

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All starting materials were purchased from commercial suppliers and used without further purification. The purities of the final compounds were characterized by high-performance liquid chromatography (LC/MS) using a gradient elution program (Ascentis Express Peptide C18 column, acetonitrile/water 5/95/95/5, 5 min, 0.05%trifluoracetic acid) and UV detection (254 nM). The purities of final compounds were 95% or greater. NMR spectra was recorded on a Bruker NMR 400 MHz Avance III spectrometer operating at 400 MHz for 1H NMR and 100 MHz for 13C NMR. Chemical shifts are given in part per million (ppm) relative to the deuterated solvent residual peak, coupling constants J are given in Hertz.
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2

Kinetic Study of Anthracene Dimerization

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The sealed capillary tube was positioned into a pre-tuned EPR-resonator equipped with a 120 mm (length) x 3 mm (OD) EPR-tube for reproducible runs. An EPR benchtop SPINSCAN-X spectrometer (ADANI, Minsk, BLR) operating at the CW X-band, modulation amplitude = 0.010 mT (0.10 G), and microwave power = 100 mW was employed in this work. The ability of the EPR spectrophotometer to auto-tune and auto-gain allowed for a better signal-to-noise ratio, lower detection limit, and a linear correlation between spin quantity and p2p intensity. The temperature dependence of the reaction in the range between 15 to 40 °C was investigated using a temperature control setup capable of maintaining the temperature of the EPR-sample within ±0.02 °C. Detailed information about the temperature controller, sample holder, and procedure adopted to minimize the temperature gradient across the sample has been described previously [23 ]. On the other hand, anthracene chloroform solution or the collected portion of the reaction mixture transferred into a regular 5-mm NMR tube was used directly for the NMR experiment. 1H-NMR spectroscopy was performed for in situ monitoring of dimer formation and characterization of the product and the monomer anthracene using a Bruker NMR 400 MHz Avance III spectrometer (Bruker Corporation, Billerica, MA, USA).
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3

Purification and Characterization of Compounds

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All materials were purchased from commercial suppliers and used without further purification. Purification was done by Reveleris X2 flash chromatography. The purities of the final compounds were characterized by high-performance liquid chromatography (HPLC) using a gradient elution program (Ascentis Express Peptide C18 column, acetonitrile/water 5/95 → 95/5, 5 min, 0.05% trifluoracetic acid) and UV detection (254 nM). The purities of final compounds were 95% or greater. NMR spectra was recorded on a Bruker NMR 400 MHz Avance III spectrometer operating at 400 MHz for 1H NMR and 100 MHz for 13C NMR. Chemical shifts are given in part per million (ppm) relative to tetramethylsilane (TMS), coupling constants J are given in Hertz. High-resolution mass spectra were obtained using electrospray ionization on a Bruker 12 T APEX-Qe FTICR-MS with an Apollo II ion source at the COSMIC Laboratory facility at Old Dominion University, VA.
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4

Compound Purification and Characterization

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All materials were purchased from commercial suppliers and used with no extra purification. The final compounds' purities were elucidated by tandem mass spectrometry (LC/MS) using a gradient elution system (acetonitrile/water 5/95/95/5, 5 min, 0.05% formic acid) on Ascentis Express Peptide C18 column, and UV detection (254 nm). The final compounds' purities were 95% or greater. A Bruker NMR 400 MHz Avance III spectrometer operating at 100 MHz for 13C NMR and 400 MHz for 1H NMR was utilised for NMR spectra recording. Chemical shifts are given relative to tetramethylsilane (TMS) in part per million (ppm), and coupling constants J are given in Hertz. HPLC-HRMS analyses were carried out using Agilent (Santa Clara, CA) 1200 series binary pump (G1312B), and columns waters XTerra MS C18 (3.5 um; 2.1 × 150 mm) + Phenomenex C18 security guard column (2 × 4 mm) on gradient elution mobile phase using 0.2% acetic acid in H2O/methanol; wavelength = 254 nm. Elemental analyses were established at Microanalytical Centre, Faculty of Science, Cairo University, Egypt using Manual Elemental Analyser Heraeus (Germany) and Automatic Elemental Analyser CHN Model 2400 Perkin Elmer (USA).
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5

Characterization of Synthesized Compounds

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All starting materials were purchased from commercial suppliers and used without further purification. The purities of the final compounds were characterized by high-performance liquid chromatography (LC/MS) using a gradient elution program (Ascentis Express Peptide C18 column, acetonitrile/water 5/95/95/5, 5 min, 0.05% trifluoracetic acid) and UV detection (254 nM). The purities of final compounds were 95% or greater. 1H NMR spectra was recorded on Varian 500 MHz operating at 500 MHz for 1H NMR and 13C NMR spectra was recorded on a Bruker NMR 400 MHz Avance III spectrometer operating at 100 MHz for 13C NMR. Chemical shifts are given in part per million (ppm) relative to the deuterated solvent residual peak, coupling constants J are given in Hertz.
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6

NMR Analysis of HEP10 Compound

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About 60 mg HEP10 powder was dissolved in 1 mL D2O and freeze dried twice. Then the residue was dissolved in 600 µL D2O and analyzed by AVANCE III 400 MHz NMR spectrometer (Bruker, Karlsruhe, Germany).
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7

Characterization of EV-Based Composite Materials

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The XRD data of EV‐Br2, Na‐AQ, and EV‐AQ2 composites were collected on a Rigaku MiniFlex600 XRD Instrument equipped with Cu Kα radiation. The scanning rate was 2° min−1, and 2θ was set between 10° and 80°. The Raman measurements were carried out through Xplora with the incident laser of 532 nm in 500–1800 cm−1. The morphology and microstructure of these materials were investigated by a Zeiss Sigma 500 SEM apparatus. The elemental mapping was performed with energy‐dispersive X‐ray spectroscopy (EDS) attached to the SEM. A thermogravimetric analyzer was used to determine the thermal stability of composites on STA 409 PC Simultaneous Thermal Analyzer with a temperature range between 30 and 900 °C at 10 °C min−1 rate, under argon condition. FTIR absorption spectra were collected to on NEXUS 470 FTIR spectrometer. The scanning region is from 100 to 4000 cm−1. NMR spectroscopy was carried out on a Bruker Avance III 400 MHz NMR spectrometer.
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8

Spectroscopic Analysis of β-Cyclodextrin Derivatives

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The Fourier transform infrared (FT-IR) spectra of β-CD, β-CDP, DS, and DS/β-CDP were collected in the range of 400–4000 cm−1 using a Fourier transform infrared spectrometer (Nicolet-IS50, Thermofisher Nicolet, New York, StateofNewYork, USA) at room temperature. The 1H NMR spectra of DS, β-CDP, and DS/β-CDP were recorded on 1H NMR (9.4 T Bruker Avance III 400 MHz NMR spectrometer, Billerica, Massachusetts, Germany)at 25 °C in D2O. The UV–Vis spectra of DS, β-CDP, and DS/β-CDP were detected using a UV–Vis spectrophotometer (Cary 5000, Agilent, Palo Alto, CA, USA).
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9

Lipid Classes Distribution by NMR

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Distribution of the lipid classes was performed by 1H NMR according to Caligiani et al. (2019) (link). NMR spectra were registered on a Bruker Avance III 400 MHz NMR Spectrometer (Bruker BioSpin, Rheinstetten, Karlsruhe, Germany) operating at a magnetic field-strength of 9.4 T.
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10

Starch Branching Degree Measurement

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The branching degree of starch was measured using the AVANCE III 400 MHz NMR Spectrometer (Bruker, karlsruhe, Switzerland) according to the method of Boonna [15 (link)].
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