13C and 1H NMR spectra were recorded at 100 and 400 MHz, respectively, on a Jeol JNM ECX-400 spectrometer (Jeol Ltd., Tokyo, Japan) using CDCl3 (50 mg/0.6 mL) as the solvent at 25 °C. As reference signals for the correction of the scale of chemical shifts, we used the signals of residual protons of the solvent (δ = 7.26 ppm) and carbon atoms of CDCl3 (δ = 77.16 ppm) for the 1H and 13C nuclei, respectively, as presented in [57 (link)].
Jnm ecx400 spectrometer
Manufactured by JEOL
Sourced in Japan
The JNM-ECX400 spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical and research applications. It operates at a frequency of 400 MHz and is capable of performing various NMR experiments to analyze the chemical and structural properties of materials.
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Lab products found in correlation
Av600 nmr instrument, by Bruker (1 mentions)
Silica gel 60n, by Kanto Chemical (1 mentions)
Jms 700 mstation spectrometer, by JEOL (1 mentions)
Spiraltof jms s3000 spectrometer, by JEOL (1 mentions)
V 670 uv vis nir spectrophotometer, by Jasco (1 mentions)
Jnm ecz600r spectrometer, by JEOL (1 mentions)
2400 2 chns o analyzer, by PerkinElmer (1 mentions)
Gcms qp2010 se, by Shimadzu (1 mentions)
Nicolet is10 spectrometer, by Thermo Fisher Scientific (1 mentions)
Ecs 400 spectrometer, by JEOL (1 mentions)
Lct premier xe, by Waters Corporation (1 mentions)
Dip 1000 polarimeter, by Jasco (1 mentions)
J 720w spectropolarimeter, by Jasco (1 mentions)
Ft ir 4200 spectrometer, by Jasco (1 mentions)
V 730bio spectrophotometer, by Jasco (1 mentions)
Gsx 400 spectrometer, by JEOL (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Direct q 3 uv, by Merck Group (1 mentions)
Lcms 2020 spectrometer, by Shimadzu (1 mentions)
15 protocols using jnm ecx400 spectrometer
1
NMR Spectroscopy Protocol: CDCl3 Solvent
2
NMR Characterization of EPS Hydrolysis
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1Н and 13C NMR spectra of the hydrolyzed EPS were recorded using a JEOL JNM-ECX400 spectrometer (JEOL, Japan) (400 and 100 MHz respectively) in a D2O/H2O solution (60 mg of substance in 0.7 ml D2O and 0.005 ml acetonitrile) with and without 70% HClO4. The signals (δH 2.06 ppm, δC 119.68 and 1.47 ppm) of acetonitrile were used as a chemical shift reference. The spectra were processed using the software packages ACD/NMR Processor Academic Edition, ver. 12.01 and Delta 4.3.6. The NMR spectra of the native polysaccharide were recorded using a Bruker AV600 NMR instrument (600 MHz) at 40°C with HDO signal suppression. To prepare the NMR sample, 20 mg of the polysaccharide were lyophilized and dissolved in 99.9% D2O. The NMR spectra were processed by MestreLabs Mestre Nova software and referenced to internal DSP at δH 0.00, δC -1.59.
3
NMR Diffusion Measurements of Compounds
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Sample solutions were prepared by dissolving each compound in CDCl3 to achieve a target concentration of 1, 5, 10, 20 or 100 mM. All the solutions were warmed at 60 °C for 10 min in a vial to ensure complete dissolution of the compounds, and equilibrated at room temperature at least 30 min before the measurement. Each solution was transferred to a micro NMR tube with the glass magnetic susceptibility matched to chloroform (Shigemi, BMS-005J). The solution height was adjusted to be 10 mm in the 5 mm O.D. tube. The spectra were recorded on a JEOL JNM-ECX400 spectrometer at the resonance frequency of 399.7822 MHz for 1H. The temperature was regulated at 25 °C and no spin was applied during measurements. All the experiments were performed using the bipolar pulse longitudinal eddy current delay (BPP-LED) sequence with spoil gradients applied during the diffusion and eddy current decay periods. The gradient duration was 1 ms and the diffusion time was within the range of 80–100 ms. The gradient strength was varied at even interval on a log-2 scale from 3 to 270 mT m−1 in 14 steps. DOSY spectra were generated by the JEOL’s native program Delta, using the adapted CONTIN algorithm for inverse Laplace transforms to build the diffusion dimension.
4
NMR Analysis of HFPS-F4 in D2O
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HFPS-F4 (30 mg) was dissolved in D2O (1 mL) in a NMR tube and analyzed in JEOL JNM-ECX400 spectrometer (Japan) and the chemical shifts were expressed in parts per million (ppm) [21 (link)].
5
Characterization of Polyphenylene Sulfide Films
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The 1H and 13C NMR
spectra were documented on a JEOL JNM-ECX400 spectrometer at resonant
frequencies of 400 MHz for 1H and 100 MHz for 13C nuclei using CDCl3-d1, THF-d8, and DMSO-d6 as
solvents and tetramethylsilane as the reference. FT-IR spectra were
recorded on a Nicolet iS5 Fourier transform spectrophotometer. Mn and Mw values
were measured by size-exclusion chromatography (SEC) on a JASCO GULLIVER
1500 system equipped with two polystyrene gel columns (Plegel 5 μm
MIXED-C) that were eluted with THF at a flow rate of 1.0 mL/min and
calibrated by polystyrene standard samples. TG measurements were performed
on a Seiko EXSTAR 6000 TG/DTA 6300 thermal analysis system at a heating
rate of 10 °C/min. DSC analysis was conducted on a DSC 6200 at
a heating rate of 10 °C/min under nitrogen. The in-plane (nTE) and out-of-plane (nTM) refractive indices of PPS films were measured using a prism
coupler (Metricon, model PC-2010) equipped with laser diodes (wavelength:
636, 845, 1324, and 1558 nm) and a half-waveplate in the light path.
The in-plane/out-of-plane birefringence values (Δn) were estimated as the difference between nTE and nTM, and the average refractive
indices were calculated according to the following equation: nav = [(2nTE2 + nTM2)/3]1/2.
spectra were documented on a JEOL JNM-ECX400 spectrometer at resonant
frequencies of 400 MHz for 1H and 100 MHz for 13C nuclei using CDCl3-d1, THF-d8, and DMSO-d6 as
solvents and tetramethylsilane as the reference. FT-IR spectra were
recorded on a Nicolet iS5 Fourier transform spectrophotometer. Mn and Mw values
were measured by size-exclusion chromatography (SEC) on a JASCO GULLIVER
1500 system equipped with two polystyrene gel columns (Plegel 5 μm
MIXED-C) that were eluted with THF at a flow rate of 1.0 mL/min and
calibrated by polystyrene standard samples. TG measurements were performed
on a Seiko EXSTAR 6000 TG/DTA 6300 thermal analysis system at a heating
rate of 10 °C/min. DSC analysis was conducted on a DSC 6200 at
a heating rate of 10 °C/min under nitrogen. The in-plane (nTE) and out-of-plane (nTM) refractive indices of PPS films were measured using a prism
coupler (Metricon, model PC-2010) equipped with laser diodes (wavelength:
636, 845, 1324, and 1558 nm) and a half-waveplate in the light path.
The in-plane/out-of-plane birefringence values (Δn) were estimated as the difference between nTE and nTM, and the average refractive
indices were calculated according to the following equation: nav = [(2nTE2 + nTM2)/3]1/2.
6
Spectroscopic Characterization of Organic Compounds
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Commercially available reagents and solvents for syntheses were of reagent grade and used without further purification. TLC and gravity column chromatography were performed on Art. 5554 (Merck KGaA, Darmstadt, Germany) plates and silica gel 60N (Kanto Chemical, Chuo, Japan), respectively. For spectral measurements, spectral-grade dichloromethane was purchased from Nacalai Tesque. 1H- and 13C-NMR spectra were recorded with a JNM-ECX 400 spectrometer JEOL Akishima, Japan) at ambient temperature using tetramethylsilane (TMS) as an internal standard. Electrospray ionization (ESI) mass spectra were recorded on a JEOL JMS-MS T100LC spectrometer. Matrix assisted laser desorption/ionization (MALDI)-TOF-MS spectra were recorded on a JEOL SpiralTOF JMS-S3000 spectrometer (JEOL Akishima, Japan). FAB mass spectra were measured on a JEOL JMS-700 MStation spectrometer. UV-vis spectra were measured using a V-670 UV/VIS/NIR Spectro-photometer (JASCO, Hachioji, Japan). The fluorescence spectra were measured with a HORIBA (Kyoto, Japan) Jobin Yvon Spectrofluorometer Fluorolog-3 (Model: FL3-11-NIR).
7
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.
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.
8
Detailed Characterization of Organic Compounds
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All starting materials and dehydrated solvents were purchased from Wako Pure Chemical Industries (Osaka, Japan) and Tokyo Chemical Industry (Tokyo, Japan). CO2 (>99.999%, H2O < 5 ppm) was obtained from Yamagata Sanso (Yamagata, Japan). The NMR spectra were obtained using a JEOL ECS-400 spectrometer operating at 400 MHz for 1H and 100 MHz for 13C. The elemental analyses were performed by a Perkin Elmer 2400II CHNS/O Analyzer. Mass spectroscopy was performed on a Shimadzu GCMS-QP2010SE in electron ionization (EI) mode. FTIR spectra were recorded on a Thermo Scientific Nicolet iS10 spectrometer equipped with a Smart iTR diamond ATR sampling accessory in the range of 4000–650 cm−1. Solid-state NMR, 13C cross-polarization (CP)/magic angle spinning (MAS, 99.5 MHz) measurements were performed on a JEOL JNM-ECX 400 spectrometer, at a spinning speed of 10 kHz. Thermogravimetric analysis (TGA) was performed on a Seiko Instrument TG-DTA 6200 using an aluminum pan in the temperature range of 30–350 °C at a heating rate of 5 °C/min under a nitrogen atmosphere (flow rate 200 mL/min). Geometry optimized energy for 1 , 2 and 3 was estimated by using DFT calculation with B3LYP/6-31G* method (Wavefunction, Inc., Spartan’06 Windows version 1.1.0) [41 (link)].
9
Spectroscopic Analysis of Chemical Compounds
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Optical rotations were measured using a JASCO DIP-1000 polarimeter. UV spectra were recorded on a JASCO V730-BIO Spectrophotometer. CD spectra were measured using a JASCO J-720 W spectropolarimeter. IR spectra were recorded on a JASCO FT/IR-4200 spectrometer. All NMR data were recorded on a JEOL JNM-ECX400 spectrometer for 1H (400 MHz) and 13C (100 MHz). 1H NMR chemical shifts (referenced to residual CHCl3 observed at δH 7.26) were assigned using a combination of data from COSY and HMQC experiments. Similarly, 13C NMR chemical shifts (referenced to CDCl3 observed at δC 77.16) were assigned based on HMBC and HMQC experiments. HRESIMS spectra were obtained on an LCT premier XE time-of-flight (TOF) mass spectrometer (LCT premier XE; Waters). Reverse-phase HPLC was performed (500 × 10 mm I.D. ODS AQ-325; YMC Co., Ltd., Kyoto, Japan), eluted at a flow rate of 1.5 mL/min with 45% (v/v) aqueous methanol, and detected at wavelength 220 nm.
10
Solid-State 13C NMR Spectroscopy
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13C NMR spectra were recorded on a JEOL JNM-ECX400 spectrometer (9.39 T, 100.5 MHz) in the solid phase at room temperature using the cross-polarization technique (CPMAS) with a rotation speed of 10 kHz in 7 mm zirconia rotors. The magic angle spinning (MAS) of the sample was determined at a rotation speed of 10 kHz. All MAS experiments were performed at room temperature; proton decoupling was performed using two-pulse phase modulation (TPPM). When registering the 13C MAS NMR spectra, rotary synchronization of the rapid spin echo (RSE) sequence or single pulse (SP) excitation at a Larmor frequency of 100.6 MHz was used. To optimize the spectrum registration process, the relaxation time of carbon nuclei was selected. The pulse duration for the 90° angle was 6 ms, and for 180°, it was 12 ms, and the total number of scans was 256. The spectra were processed using the ACD/NMR Processor Academic Edition, Ver. 12.01.
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