One-dimensional spectra on 10 mg of dry sample exchanged in dimethyl sulfoxide-d6, 99.9% containing 0.05 v/v TMS (Wako, Japan) were acquired using a Jeol 600 MHz instrument. The operation conditions for 1H NMR were as follows: spin, 15 Hz; relaxation delay, 5 s; temperature, 25°C.
600 mhz instrument
Manufactured by JEOL
Sourced in Japan
The 600 MHz instrument is a high-performance nuclear magnetic resonance (NMR) spectrometer capable of operating at a frequency of 600 MHz. It is designed to analyze the molecular structure and composition of various samples through the detection and measurement of nuclear magnetic resonances.
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Lab products found in correlation
3 protocols using 600 mhz instrument
1
1D NMR Spectroscopy of Dry Samples
2
Quantitative 1H NMR for Ammonia Analysis
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1H NMR spectra were provided by using a 600-MHz instrument
(JEOL)
available at the Freie Universität of Berlin. In a typical
measurement for ammonia quantification, 10 mL of the used electrolyte
solution were added to a clean glass vial containing 5.0 mg of maleic
acid used as an internal standard (ReagentPlus, ≥99% (HPLC),
Sigma-Aldrich), followed by the addition of 2.5 mL H2SO4 4 M to acidify the mixture. After ensuring complete miscibility,
the nuclear magnetic resonance tube was filled by mixing 500 μL
of the mixture and 50 μL of deuterium oxide (D2O,
99.9 atom %D, Sigma-Aldrich). The concentration of 14NH4+/15NH4+ in the
samples was derived from the integral ratio of the triplet/doublet
ammonium signal and the singlet of the maleic acid standard. Standard
solutions with known 14NH4Cl (99.998%, Sigma-Aldrich)
and 15NH4Cl (Sigma-Aldrich, ≥98 atom
% 15N, ≥99%) concentration were used to construct
calibration curves for 14NH4+ and 15NH4+ determination, respectively.
(JEOL)
available at the Freie Universität of Berlin. In a typical
measurement for ammonia quantification, 10 mL of the used electrolyte
solution were added to a clean glass vial containing 5.0 mg of maleic
acid used as an internal standard (ReagentPlus, ≥99% (HPLC),
Sigma-Aldrich), followed by the addition of 2.5 mL H2SO4 4 M to acidify the mixture. After ensuring complete miscibility,
the nuclear magnetic resonance tube was filled by mixing 500 μL
of the mixture and 50 μL of deuterium oxide (D2O,
99.9 atom %D, Sigma-Aldrich). The concentration of 14NH4+/15NH4+ in the
samples was derived from the integral ratio of the triplet/doublet
ammonium signal and the singlet of the maleic acid standard. Standard
solutions with known 14NH4Cl (99.998%, Sigma-Aldrich)
and 15NH4Cl (Sigma-Aldrich, ≥98 atom
% 15N, ≥99%) concentration were used to construct
calibration curves for 14NH4+ and 15NH4+ determination, respectively.
3
NMR Characterization of Exchanged Samples
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The one-dimensional spectra, on 4-50 mg of dry, exchanged samples in deuterium oxide (0.6 ml, 99.9 atom%) with 3-(trimethylsilyl) propionic acid-d 4 sodium salt (internal standard), were recorded using a Jeol 600 MHz instrument. The operation conditions for one-dimensional spectra were as follows: 1-H NMR; spin, 15 Hz; relaxation delay, 2 s; acquisition, 1000 scans; temperature, 30 °C: 13-C NMR; spin, 15 Hz; relaxation delay, 2 s; acquisition, 33 000 scans; temperature, 30 °C. The water resonance was suppressed by selective irradiation during the relaxation delay.
The two-dimensional spectra were obtained by using COSY, NOESY and TOCSY functions. The operation conditions for two-dimensional spectra were as follows: COSY; spin, 15 Hz; acquisition, 16 proton scans; acquisition, 128 COSY scans; temperature, 30 °C: NOESY; mixing time, 150 ms; acquisition, 40 proton scans; acquisition, 40 NOESY scans; temperature, 30 °C: TOCSY; spin, 15 Hz; acquisition, 16 proton scans; acquisition, 64 TOCSY scans; spin locking, MLEV17; temperature, 30 °C.
The two-dimensional spectra were obtained by using COSY, NOESY and TOCSY functions. The operation conditions for two-dimensional spectra were as follows: COSY; spin, 15 Hz; acquisition, 16 proton scans; acquisition, 128 COSY scans; temperature, 30 °C: NOESY; mixing time, 150 ms; acquisition, 40 proton scans; acquisition, 40 NOESY scans; temperature, 30 °C: TOCSY; spin, 15 Hz; acquisition, 16 proton scans; acquisition, 64 TOCSY scans; spin locking, MLEV17; temperature, 30 °C.
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