Reagents were obtained from commercial suppliers and were used without purification, except for ethyl formate which was distilled before use. Standard syringe techniques were used to transfer dry solvents and air‐ or moisture‐sensitive reagents. Reactions were followed, and RF values were obtained using thin‐layer chromatography (TLC) on silica gel‐coated plates (Merck 60 F254) with the indicated solvent mixture. Detection was performed under ultraviolet (UV) light and by charring at ∼ 150 °C after dipping into a solution of either 2% anisaldehyde in ethanol/H2SO4, KMnO4 or ninhydrin. Nuclear magnetic resonance (1H and 13C NMR) spectra were recorded at 298 K on a Varian Inova 400 (400 MHz), Bruker Avance III 400 MHz or Bruker Avance III 500 MHz spectrometer in the solvent indicated. Chemical shifts are given in parts per million (ppm) with respect to tetramethylsilane (0.00 ppm) as the internal standard for 1H NMR and CDCl3 (77.16 ppm) as the internal standard for 13C NMR. Coupling constants are reported as J values in hertz (Hz). High‐resolution mass spectra (HRMS) were recorded with JEOL AccuTOF mass spectrometer. Column or flash chromatography was carried out using ACROS silica gel (0.035–0.070 mm and 60 Å pore diameter).
Accutof mass spectrometer
Manufactured by JEOL
Sourced in Japan, United States
The AccuTOF mass spectrometer is a high-resolution time-of-flight mass spectrometer manufactured by JEOL. It is designed to provide accurate mass measurement and high-performance analysis of a wide range of samples.
Automatically generated - may contain errors
Lab products found in correlation
Inova 400, by Bruker (1 mentions)
Avance 3 400 mhz, by Bruker (1 mentions)
Accutof lc plus jms t100lp mass spectrometer, by JEOL (1 mentions)
Peg1000, by Merck Group (1 mentions)
Mercury 400 mhz spectrometer, by Agilent Technologies (1 mentions)
Unityplus 500 mhz, by Agilent Technologies (1 mentions)
4 protocols using accutof mass spectrometer
1
Purification and Characterization of Compounds
2
Isothermal Decomposition of PMMA
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The isothermal decomposition of PMMA was analyzed with an Accu-ToF LC-plus JMS-T100 LP mass spectrometer JEOL (Tokyo, Japan) working with a direct-analysis-in-real-time (DART) ion source (Ion Sense, Saugus, MA, USA). The sample was used without any prior preparation. The fragments that resulted from the decomposition process were evaporated in a stream of helium atmosphere heated at constant temperatures of 200, 250, 300, 350, 400, 450, 500 and 550 °C. The heated helium/vapor mixture was then ionized by excited metastable helium atoms before entering the ion source of the time-of-flight mass spectrometer. All the samples were analyzed with DART-ToF-MS using the Accu-TOF mass spectrometer acquired from JEOL (Tokyo, Japan). The experimental conditions were as follows: vacuum level 1.3 × 105 Pa, He used as a heating and ionization gas, ring lens with a voltage of 4 V, peaks voltage of 500 V, and a mass resolution that ranged between 3600 and 4900. The sample (1–2 mg) in powder form was placed in a small piece of sandpaper and introduced between the DART outlet and the MS port inlet, and polyethylene glycol (104 g·mol−1) was used in this work for calibration.
3
DART-TOF-MS Analysis of Herbal Products
4
Analytical Techniques for Chemical Characterization
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All commercial materials (solvents, reagents, and substrates) were used as received. SilicaFlash silica gel, P60, 40–63 µm particle size (SiliCycle) was used for column chromatography. High-performance liquid chromatography was performed on a PerkinElmer Series 200 pump with a Waters 2487 Dual λ Absorbance Detector connected to an eDAQ PowerChrom 280 recorder. One-dimensional 1H and 13C NMR spectra were recorded on a Varian UnityPlus 500 MHz or Varian Mercury 400 MHz spectrometer. Chemical shifts are reported in ppm, and the signals were referenced to residual undeuterated solvent signals. Mass spectra were recorded using an Agilent 6538 mass spectrometer with a Q-TOF ionization source or a JEOL AccuTOF mass spectrometer with a DART ionization source.
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