BARBOSA, L. L.

COLNAGO, L. A.

MAZO, L. H.

Nunes, L. M. S.

RCAAP - Repositório Científico de Acesso Aberto de Portugal

Use of SSFP C NMR to monitor in situ electrochemical reaction in spectroelectrochemical cell

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WWMR2010Joint EUROMAR 2010and 17th ISMAR ConferenceBook of AbstractsFlorence, July 4-9,20107. PostersP643Use of SSFP 13C NMR to monitor in situ electrochemical reaction inspectroelectrochemical cellLuiza M. S. Nunesa, Lúcio L. Barbosa", Luiz H. Mazo" and Luiz A. Colnago"~CInstitute ofChemistry ofSão Carlos, University ofSão Paulo, 400 Trab.São-carlense St, 13560-970, São Carlos-SP, Brazil (!.uizanunes@iqs,· "'/' /011bFederal University of Espírito Santo, 514 Fernando Ferrari St, 29075-910, Vitória - ES, BrazildEMBRAPA Agricultural Instrumentation, 1452 XV de Novembro St, 13560-970, São Carlo - SP, BrazilThe main advantage in situ measurements, which couple, electrochemistry techniques (EC) and nuclear 111:1/',IIl'11Iresonance spectroscopy (NMR) is obtain information in real time about electrogenerated species, in solution. Moxr I (NMR studies uses the IH NMR detection to monitor the electrochemical processes due toIH high sensitivity and fast data acquisition.l'" To obtain I3C spectra faster spectrum thanconventional I3C NMR sequence to monitor in situ the electrolysis's reaction(organochloride reduction) we examined the application of I3C Steady State FreePrecession sequence (SSFP). Figure 1 shows the diagram of EC-NMR cell assembled ina 10 rnm NMR tube. The spectroelectrochemical cell contains the three electrodes, thereference, working and counter electrodes. The in situ electrochemical reaction wasperformed with potentiostat coupled in the cell placed inside the high-field NMRspectrometer. The I3C SSFP measurements were performed for 10 minutes during theelectrochemical reaction. The signal to noise enhanced provided by SSFP sequence demonstrates by fust time 11111possibility of in situ monitoring of I3CNMR in spectroeletrochemical study.References:I. Webster R. D., Analytical Chemistry, 76, 1603 - 1610 (2004)2. Klod S., Ziegs F. and Dunsch L., Analytical Chemistry, 81, 10262 - 10267 (2009)Acknowledgments: FAPESP, EMBRAPA Agricultura! Instrumentation.P644Assignment of the Proton and Carbon-13 Resonances of an unsymmetrical beta-Cyclodextrin DerivativeBertrand Plainchont", Agathe Martinez a, Severine Tisseb, Jean-Philippe Bouillon", Jean-MichelWieruszeski", Guy Lippens", Damien Jeanneratd and Jean-Marc Nuzillard""Institut de Chimie Moléculaire de Reims, Université de Reims-Champagne-Ardenne, 51687 Reims, France Om.nuzillard@univ-reims.fr)bSciences et Méthodes Séparatives, IRCOF, Université de Rouen, 76821 Mont-Saint-Aignan Cedex, France"Groupe JU.DI et Modélisation molécula ire, Université de Lille, 59655 Vil/eneuve d'Ascq Cedex, France"Département de Chimie Organique, Université de Genêve, CH-1211 Genêve 4, SuisseCompound 1 is a starting material in the synthesis of chiralstationary phases for gas chromatography.' The assignment ofits IH andI3C sugar resonances was achieved by means of new and conventionalpulse sequences.The sequential assignment ofthe sugar units was obtained using a FIdecoup'led FI band-selective 2D TOCSY - ROESY experirnent. The IHand I C resonances in each sugar unit were assigned by means ofsensitivity optimized 3D TOCSY - DQFCOSY and TOCSY - HSQCspectra, of FI band-selective 2D HSQC - RELA Y and of aliased 2DHSQC - TOCSy2 spectra.References:l. Stephany o., Dron F., Tisse S., Martinez A., Nuzillard J.-M., Peulon-Agasse V.,Cardinaêl P. and Bouillon J.-P., J Chromatogr. A, 1216,4051 - 4062 (2009)2. Vitorge B., Bieri S., Humam M., Christen P., Hostettmann K., Munoz O., Loss S. andJeannerat D., Chem. Commun., 950 (2009)4681

Use of SSFP C NMR to monitor in situ electrochemical reaction in spectroelectrochemical cell.

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Use of SSFP C NMR to monitor in situ electrochemical reaction in spectroelectrochemical cell

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