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Precise measurement of 1H 90° pulse in solid-state NMR spectroscopy for complex and heterogeneous molecular systems

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Abstract

The 90° pulse calibration is essential in NMR spectroscopy to prevent artefacts in the liquid state or to enhance cross-polarization efficiency in the solid state. We verified pulse-angle (PA) errors due to circuit impedances in solid-state NMR and suggested a possible solution to prevent the inconvenience of PA errors. The classic pulse sequences used to calibrate 1H 90° pulse lengths by direct detection of protons or by cross-polarization were modified in order to replace single 1H pulses with 1H pulse trains. Pulse trains were found to decrease the effect of PA imperfections in the calibration of basic pulses (i.e. 90° and 180°) for a number of organic substrates. The modified sequences are especially important to rapidly obtain pulse calibration of complex and heterogeneous molecular systems such as humic substances, which usually require a long time when using single 1H pulses.

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Acknowledgements

The authors gratefully acknowledge a fruitful discussion with Francesca Benevelli from Bruker Biospin, Italy, and the help of Daniela Šmejkalová (Università di Napoli Federico II) in evaluation of spectra.

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Authors and Affiliations

  1. Dipartimento di Ingegneria e Tecnologie Agro-Forestali (DITAF), Università di Palermo, Viale delle Scienze 13, 90128, Palermo, Italy

    Pellegrino Conte

  2. Centro di Ricerca Interdipartimentale per la Spettroscopia di Risonanza Magnetica Nucleare (CERMANU), Facoltà di Agraria, Università di Napoli Federico II, Via Università 100, 80055, Portici, Italy

    Pellegrino Conte & Alessandro Piccolo

  3. Dipartimento di Scienze del Suolo, della Pianta, dell’Ambiente e delle Produzioni Animali (DiSSPAPA), Università di Napoli Federico II, Via Università 100, 80055, Portici, Italy

    Alessandro Piccolo

Authors
  1. Pellegrino Conte
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  2. Alessandro Piccolo
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Correspondence to Pellegrino Conte.

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Conte, P., Piccolo, A. Precise measurement of 1H 90° pulse in solid-state NMR spectroscopy for complex and heterogeneous molecular systems. Anal Bioanal Chem 387, 2903–2909 (2007). https://doi.org/10.1007/s00216-007-1156-8

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  • DOI: https://doi.org/10.1007/s00216-007-1156-8

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