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Jnm ecz600r spectrometer

Manufactured by JEOL
Sourced in Japan

The JNM-ECZ600R spectrometer is a powerful NMR (Nuclear Magnetic Resonance) instrument designed for advanced analytical applications. It features a 600 MHz superconducting magnet and delivers high-resolution NMR spectroscopy capabilities. The spectrometer is capable of performing various NMR experiments to analyze the chemical structure and properties of samples.

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15 protocols using jnm ecz600r spectrometer

1

Quantitative 31P and 7Li NMR Spectroscopy

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31P magic-angle spinning (MAS) NMR spectroscopy using dry air
was performed with a JEOL JNM-ECX400 spectrometer (9.4 T) with a 4
mm MAS probe. The 31P MAS NMR spectra were collected at
a spinning frequency of 15 kHz with a π/2 excitation pulse of
3.11 μs. A total of 32 scans with a 60 s recycle delay were
used to ensure good quantitative peak intensities. The chemical shifts
of the 31P MAS NMR spectra were referenced to an 85% H3PO4 solution (0 ppm).
7Li MAS
NMR spectroscopy was performed by using a JEOL JNM-ECZ-600R spectrometer
(14.1 T) with a 3.2 mm MAS probe. The 7Li MAS NMR experiments
were performed with a 20 kHz spinning speed and a 2.90 μs excitation
pulse. The delay time between each of the eight scans was set to 60
s to ensure good quantitative peak intensities. A 1 M LiCl solution
was used for the chemical shift reference (0 ppm).
For the solid-state 31P and 7Li NMR measurements,
the samples were packed into ZrO2 sample tubes in a glovebox.
No spectral changes were observed during the NMR measurements, meaning
that the use of airtight sample tubes prevented reactions with oxygen
and water in the air.
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2

Antioxidant Characterization of Novel Compounds

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The antioxidant properties were conducted using UV/Vis spectrophotometer (UV-1800 240 V, Shimadzu, Japan). The NMR data (1H NMR at 600 MHz, 13C NMR at 150 MHz) were obtained on a JNM-ECZ600R spectrometer (JEOL, Tokyo, Japan) using deuterated solvents (CD3OD and DMSO‑d6). The HPLC system was performed by an Agilent 1200 series (Agilent Technologies, Palo Alto, CA, USA) equipped with a quaternary pump, an autosampler, a vaccum degasser, a thermal chamber controller, and a UV detector. The mass spectrometry was performed using an Ultimate 3000 LC system with a Q Exactive Focus quadrupole-Orbitrap mass spectrometer system (Thermo Fisher Scientific Inc., Waltham, MA, USA).
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3

Starch Crystallinity Analysis by NMR

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The 13C CP/MAS NMR analysis of the starch was performed on a JNM-ECZ600R spectrometer (JEOL Ltd., Tokyo, Japan); the frequency of 150.913 MHz, tube diameter of 3.2 mm, magic-angle spinning frequency of 12 kHz, relaxation delay of 2 s, and scans of 1221 were used during the experiments. The specific relative crystallinity, double helix content, and the amorphous phase were calculated according to previously established methods [27 (link),28 (link)].
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4

Comprehensive Spectroscopic Analysis of Molecular Compounds

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Attenuated total reflectance/Fourier transform infrared (ATR-FTIR) spectroscopy was performed using a Thermo Fisher Scientific Nicolet is10 infrared spectrometer with a scan range of 600–4000 cm−1 over 16 scans.
1H nuclear mangnetic resonance (1H-NMR) was performed using an AVANCE-III-500 MHz spectrometer (Bruker, Switzerland) using deuterated acetone (C3D6O) as the solvent and tetramethylsilane (TMS) as the standard.
19F-NMR was performed using an AVANCE-NEO-400 MHz spectrometer (Bruker, Switzerland), and the standard was monofluorotrichloromethane (CFCl3).
Solid-state 19F-NMR was performed using an JEOL JNM ECZ600R spectrometer (Japan), and the specific conditions were frequency of 564 MHz, pulse width of 90 deg and rotating speed of 21 kHz.
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5

Purification and Characterization of Organic Compounds

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All the reactants, reagents, and solvents were obtained from commercial sources and used without further purification. Except where noted otherwise, the reactions were performed under an inert atmosphere of nitrogen gas using anhydrous solvents. The reactions were monitored using liquid chromatography–mass spectrometry (Agilent 1290 Infinity LC, Agilent 6120 quadrupole LC/MS, Agilent, Santa Clara, CA, USA). Flash chromatography was performed using the CombiFlash® system (Teledyne Isco, St. Lincoln, NE, USA). All nuclear magnetic resonance spectra were collected using a 600 MHz JNM-ECZ600R spectrometer (JEOL, Akishima, Tokyo). Chemical shifts (d in ppm) in the 1H spectra were reported relative to the residual solvent signals: 7.26 ppm for chloroform-d.
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6

Optical Rotation and NMR Analysis

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General Experimental Procedures Optical rotation was measured using an MCP 150 module type small polarimeter (Anton Paar). The 1 H-and 13 (link) C-NMR spectra were measured using a JNM-ECZ600R spectrometer (JEOL) at 600 and 150 MHz, respectively, and the chemical shifts are reported on the δ (ppm) scale. The high resolution (HR)-FAB-MS were measured using a JEOL JMS-HX110 mass spectrometer and acquired in a glycerol matrix. HPLC was conducted using a Waters machine equipped with a 1525 binary pump and a 2489 UV/Vis detector. Separation was carried out using a Cosmosil 5C 18 MS-II column (20.0 × 250 mm, octadecyl silica (ODS), 5 µm, Nacalai Tesque, Kyoto, Japan). Apoptosis and cell cycle analyses were carried out using a Muse Cell Analyzer (Merck KGaA, Darmstadt, Germany).
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7

NMR Analysis of Compound Spectra

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1D nuclear magnetic resonance (NMR) spectra were analyzed at 600 MHz (1H-NMR) and 150 MHz (13C-NMR) using a JNM-ECZ600R spectrometer (JEOL, Tokyo, Japan). Samples were dissolved in deuterated methanol (CD3OD) and dimethyl sulfoxide (DMSO-d6). Chemical shifts are presented as ppm (parts per million) on the δ scale and coupling constants (J) are presented in Hertz.
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8

Spectroscopic Characterization of Compounds

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1H- and 13C-NMR spectra were recorded in Fourier transform mode on a JEOL JNM-ECZ600R spectrometer (JEOL Ltd, Japan) operating at a nominal frequency of 600 and 150 MHz, respectively. Samples were dissolved in deuterated dimethyl sulfoxide (DMSO-d6) unless otherwise stated. All spectra were processed using Delta NMR v5.0.5.1 software. Infrared spectra were recorded as neat samples using a Perkin-Elmer Spectrum 100 FT-IR Spectrometer (PerkinElmer, USA). All IR data were manipulated using Spectrum v6.3.5 software.
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9

Comprehensive Characterization of Hydrogel Composite

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FT‐IR spectra were recorded on a FT‐IR (Nicolet 5700, USA) using freeze‐dried hydrogel pellet (4000–500 cm−1). The surface morphology investigation was carried out on a field emission scanning electron microscope (FE‐SEM, Hitachi S4800) and energy‐dispersive spectroscopy mapping (EDS, Bruker Nano XFlash Detector 5030). Before the FE‐SEM investigation, the samples were sputtered with gold. A Kratos AXIS‐SUPRA spectrometer was used to analyze the XPS (Zetasizer Nano S90) of the materials. Powder XRD measurements were performed using Cu Kα (λ = 0.154056 nm) radiation with a scan rate of 4° min−1 and a step size of 0.03° in the 2θ range of 5° to 60°. The 1H CP/MAS NMR spectra were measured on a JEOL JNM‐ECZ‐600R spectrometer. The specific surface area of the composite material was measured through nitrogen adsorption at 77 K using a Micromeritics ASAP 2040 Analyzer in the range of the relative pressures P/P0 = 0.06–0.99 with a step of 0.015. Q500 equipment was used for TG analysis with a heating rate of 20 °C min−1 from 35 to 800 °C in the air. The transmittance of the hydrogel was measured with a commercial tester (LS116, China) at a wavelength of 550 nm.
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10

Solid-State NMR Characterization Protocols

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The ssMAS NMR measurements were performed
on a JEOL JNM-ECZ600R spectrometer with a 14.09 T magnet. 11B MAS NMR spectra were acquired using 3.2 mm MAS NMR probes with
a spinning rate of 20 kHz. The chemical shifts were referenced to
a 1 mol/L H3BO3 aqueous solution at 19.6 ppm. 1H MAS NMR spectra were obtained using a 3.2 mm MAS NMR probe
with a spinning rate of 15 kHz. The chemical shifts were referenced
to tetramethylsilane. 29Si MAS NMR experiments were recorded
using an 8 mm MAS probe with a spinning rate of 6 kHz.
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