1H and 13C NMR spectra were recorded at 25 °C on a Bruker model AC-500 spectrometer (Bruker, Billerica, MA, USA), operating at 500 and 125 MHz, respectively, where chemical shifts (δ in ppm) were determined with respect to non-deuterated solvent residues as internal standards. Analytical size exclusion chromatography (SEC) was performed in tetrahydrofuran (THF) at 40 °C, using 8.0 mm × 300 mm gel columns (Shodex KF-804 × 2) on a TOSOH model DP-8020 (TOSOH, Tokyo, Japan) with an RI-8022 RI detector (TOSOH, Tokyo, Japan). The number-average molecular weight (Mn) and polydispersity ratio (Mw/Mn) were calculated from the chromatographs with respect to 15 polystyrene standards (Scientific Polymer Products, Inc., Ontario, NY, USA; Mn = 580–670,000, Mw/Mn = 1.01–1.07). Elemental analyses were recorded on a Yanaco CHN CORDER MT-5 instrument (Yanaco, Tokyo, Japan). UV-vis spectra were recorded using a quartz cell of 1 cm path length on a SHIMADZU Type UV-2550 spectrometer (SHIMADZU, Kyoto, Japan).
Ac 500 spectrometer
Manufactured by Bruker
Sourced in United States
The AC-500 spectrometer is a nuclear magnetic resonance (NMR) instrument designed for analytical applications. It provides high-resolution NMR data acquisition and processing capabilities. The core function of the AC-500 is to analyze the molecular structure and properties of chemical samples through the detection and measurement of nuclear magnetic resonances.
Automatically generated - may contain errors
Lab products found in correlation
Dp 8020, by Tosoh (1 mentions)
Autoflex 3 maldi tof tof, by Bruker (1 mentions)
Ri 2031 ri detector, by Jasco (1 mentions)
Pu 2089, by Jasco (1 mentions)
Ft ir 4200 spectrometer, by Jasco (1 mentions)
2414 differential refractometer, by Waters Corporation (1 mentions)
Ac 300 spectrometer, by Bruker (1 mentions)
X500 qtof, by AB Sciex (1 mentions)
7 protocols using ac 500 spectrometer
1
Spectroscopic Characterization of Polymer Samples
2
Polymer Characterization by NMR, SEC, MALDI-TOF
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1H and 13C NMR spectra were recorded at 25 °C on a Bruker model AC-500 spectrometer (Bruker, Billerica, MA, USA), operating at 500 and 125 MHz, respectively, where chemical shifts (δ in ppm) were determined with respect to non-deuterated solvent residues as internal standards. Analytical size exclusion chromatography (SEC) was performed in 0.2 mol·L−1 NaNO3 aqueous solution at 40 °C, using 7.8 mm × 300 mm gel columns (TOSOH TSKgel α–3000 × 3) on a JASCO model PU2089 (JASCO, Hachioji, Japan) equipped with a UV-2075 variable-wavelength UV-vis detector (JASCO) and an RI-2031 RI detector (JASCO). The number-average molecular weight (Mn) and polydispersity ratio (Mw/Mn) were calculated from the chromatographs with respect to poly(ethylene glycol)s standards (Scientific Polymer Products, Inc., Ontario, NY, USA); Mn = 590−11,900 g/mol, Mw/Mn = 1.05–1.11). Matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF) mass spectrometry was performed on a BRUKER model AutoFlex III MALDI-TOF/TOF (Bruker) using 2,5-dihydroxybenzoic acid as a matrix. Fluorescence emission spectra were recorded on a JASCO Type FP-6500 spectrometer (JASCO).
3
NMR and Mass Spectrometry Characterization
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The 1H NMR and 13C NMR spectra were recorded on a Bruker AC500 spectrometer at 500 and 125 MHz, respectively, using deuterated chloroform (CDCl3) or dimethyl sulphoxide (DMSO) as solvents. The chemical shift for each signal was reported in ppm units with tetramethylsilane (TMS) as a standard internal reference. The MALDI-TOF-MS mass spectra were recorded using an AXIMA-CFRTM instrument. The compounds were characterized by using a Flash EA 1112, CHN elemental analysis instrument.
4
Synthesis and Characterization of Novel Compounds
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All commercially available reagents were used without further purification unless otherwise stated. The progress of the reactions was monitored by analytical TLC performed on Marcherey–Nagel silica gel 60 F254 plates, and the visualization, using anisaldehyde. The purification of derivatives was done using column chromatography with silica 60 matrix (70–270 mesh). Melting points were determined on melting point PFM-II Tecnopon apparatus, but they were not corrected. IR spectra through the range of 4000 to 600 cm-1 were run on a Jasco FT/IR – 4200 spectrometer. 1H and 13C NMR spectra were recorded on a Bruker AC500 spectrometer operating at 500 and 125 MHz, respectively, with tetramethylsilane as internal standard, using deuterated chloroform. Chemical shifts were expressed as values in parts per million (ppm), and the coupling constants (J) were given in hertz (Hz). Yield values correspond to purified compounds and were not optimized.
5
NMR and SEC Characterization of Polymers
6
NMR Spectroscopic Analysis Protocol
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Monodimensional and/or bidimensional
nuclear magnetic
resonance proton and carbon spectra (1H and 13C NMR, respectively) were acquired at 25 °C on a Bruker AC-300
spectrometer (300 MHz for 1H and 75.5 MHz for 13C) and a Bruker AC-500 spectrometer (500 MHz for 1H and
125.7 MHz for 13C) at the indicated temperature. Chemical
shifts (δ) are reported in parts per million relative to residual
solvent signals (CHCl3, 7.26 ppm for 1H NMR;
CDCl3, 77.16 ppm for 13C NMR), and coupling
constants (J) in hertz. The following abbreviations
are used to indicate the multiplicity in NMR spectra: s, singlet;
d, doublet; t, triplet; q, quartet; app, apparent; m, multiplet; bs,
broad signal. 13C NMR spectra were acquired in a broad
band decoupled mode using DEPT experiments (distorsionless enhancement
by polarization transfer) for assigning different types of carbon
environments. Selective nOe, NOESY, COSY, HSQC, and HMBC experiments
were acquired to confirm a precise molecular configuration and to
assist in deconvoluting complex multiplet signals.
nuclear magnetic
resonance proton and carbon spectra (1H and 13C NMR, respectively) were acquired at 25 °C on a Bruker AC-300
spectrometer (300 MHz for 1H and 75.5 MHz for 13C) and a Bruker AC-500 spectrometer (500 MHz for 1H and
125.7 MHz for 13C) at the indicated temperature. Chemical
shifts (δ) are reported in parts per million relative to residual
solvent signals (CHCl3, 7.26 ppm for 1H NMR;
CDCl3, 77.16 ppm for 13C NMR), and coupling
constants (J) in hertz. The following abbreviations
are used to indicate the multiplicity in NMR spectra: s, singlet;
d, doublet; t, triplet; q, quartet; app, apparent; m, multiplet; bs,
broad signal. 13C NMR spectra were acquired in a broad
band decoupled mode using DEPT experiments (distorsionless enhancement
by polarization transfer) for assigning different types of carbon
environments. Selective nOe, NOESY, COSY, HSQC, and HMBC experiments
were acquired to confirm a precise molecular configuration and to
assist in deconvoluting complex multiplet signals.
7
Spectroscopic Analysis of Compounds
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The NMR spectra were obtained on a BRUKER AC 500 spectrometer (500 MHz for 1 H-NMR and 125 MHz for 13 (link) C-NMR). The SCIEX X500 QTOF and X500 QTOF machines were used to record the high resolution-mass spectra and the ESI/APCI mass spectra, respectively. Column chromatography was ap-plied to the silica gel normal-phase (Kieselgel 60, 230-400 mesh, Merck). The thin-layer chromatography technique was done by using silica gel plates (Kieselgel 60 F 254 , 0.25 mm, Merck).
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