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SPECTROPOLE

Fédération des Sciences Chimiques de Marseille FR1739. SPECTROPOLE. Un Centre de Ressources Analytiques   au Service  de la Recherche et des Entreprises -. Dr. Gaëtan HERBETTE. Plan. Solution NMR Spectroscopy Solution NMR Service Solution NMR in automatic and manual mode

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SPECTROPOLE

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  1. Fédération des Sciences Chimiques de Marseille FR1739 SPECTROPOLE • Un Centre de Ressources Analytiques  •  au Service  de la Recherche et des Entreprises - Dr. Gaëtan HERBETTE

  2. Plan • Solution NMR Spectroscopy • Solution NMR Service • Solution NMR in automatic and manual mode • Contact - Form • Conclusion

  3. Nuclear Magnetic Resonance spectroscopy A nucleus is observed by NMR if exhibits magnetic properties characterized by the existence of a number of non-zero spin I : ZAX Z: proton, A: nucleon (proton+nucleon) A and Z even => I = 0. Examples are 612C, and 816O => No NMR A Odd => I = 1/2 ( 1H, 13C, 19F ), I = 3/2 ( 11B ), I = 5/2 ( 17O )... A Even and Z odd => I=1, 2... Examples are I = 1 ( 2H, 14N ). Observable Nucleus by NMR:

  4. Solution Nuclear Magnetic Resonance spectroscopy Solution Solution in a magnet Signal a time RF B0 FT Signal a frequency NMR Sequences: 1D, 2D homo / heteronucleaire, 3D NMR analysis: Table of chemical shift 1H NMR spectrum: integration of a signal is proportional to the number of protons Fine structure of the spectrum corresponds to the spin-spin coupling

  5. Plan • Solution NMR Spectroscopy • Solution NMR in automatic and manual mode • Contact - Form • Conclusion Solution NMR Service

  6. NMR Service – Spectropole, site de l’étoile • 4 liquid NMR spectrometers on Spectropole – 1 MCF, 2 Engineers • 2 liquid spectrometers with engineer : • Avance I 500, Avance III 600MHz, probe BBFO+ Autosampler  SampleXpress Lite/Sample Jet • 2 liquid spectrometers in self service : Avance III Nanobay 300-400MHz probe BBFO+, Autosampler  BACS 60/120

  7. NMR Service – Institut de Microbiologie de la Méditerranée, site Joseph Aiguier • 2 NMR liquidspectrometersacces on CNRS Joseph Aiguier • 1 spectrometer Avance III 500MHz QXI (1H, 13C, 15N, 31P) autosamplerNMR case • 1 spectrometer Avance III 600MHz Cryoprobe TCI (1H, 13C, 15N)

  8. Plan • Historique - Structure • Service de RMN • La RMN en solution en mode automatique, manuel • Contact - Form • Conclusion Solution NMR in automatic and manual mode

  9. Solution NMR Service security Regulation • Respect of safetyrules. No chemicalhandling in NMR room. • Respect rules of procedure (regulationform and recommendationsdisplayed in the room).

  10. Sample Preparation Tubes: - Different NMR tube size (1  10mm) - Routine quality up to 400MHz - Adaptedto field > 400MHz - Minimum length 17cm, clean and dry. Solution: - Sampleisdissolved in adequatedeuteriumsolvent (CDCl3, CD3OD, dmso-d6, D2O…) -Choiceof solventdepending on the solubility and experience. - Removalof suspendedparticles => homogeneousand clear solution. - Volume of solution: 600µl Calibration : Standard tube 5mm Micro-tube 2,5mm Capillary tube 12mm measuring area

  11. Solution NMR service in automatic mode • Spectrometers operating in automatic mode at 300MHz, 400MHz Login Password • Experiments: 1H, 13C, 19F, 31P, 119Sn… 1D, 2D • Visualization of programming on “IconWeb” • Downloading and data processing : - Data server sFTP - Free processing software (ACDLabs, Spinworks…) - Formations realized by Spectropole With nearly 200 users, spectrometers are available and accessibles 24H/24 et 7days/7 • Research, Quality Control, Screening... • Scope: chemical, pharmaceutical, food, natural products, polymers..

  12. Solution NMR service in manual mode (Engineer) • Spectrometers operating in manual mode at 500MHz, 600MHz • Other nuclei and non automatic programmed sequences • Experiments requiring long accumulation time • Small amount of sample • resolutionenhancement • Quantification (ERETIC) • NMR Diffusion • Kinetic • NMR analysisatdifferenttempérature ( -80 +120°C) • Metabolomic • … • Downloading and data processing : - Data server sFTP - Free processing software (ACDLabs, Spinworks…) - Formations realized by Spectropole “ Detailed “ analyzes requiring the intervention of an engineer

  13. NMR Cryoprobe 600MHz NMR analysis of very small quantities of sample This accessory has a probe connected to a cryogenic unit. The antenna and the electronics module are cooled to 20 K by liquid helium, thereby multiplying the sensitivity by about 4 (# 900MHz) Best sensitivity probe 1H, 13C, 15Nthreshold sensitivity 1H ~10 ng # 10-6M specific Preamplifiers Helium Compressor Cryogenic unit Cryoprobe

  14. Plan • Solution NMR Spectroscopy • Solution NMR Service • Solution NMR in automatic and manual mode • Contact - Form – Prices • Conclusion Contact - Form

  15. Liquid NMR – Spectropole site de L’étoile

  16. Liquid NMR – Spectropole site de L’étoile Service 511 SPECTROMETRIE DE MASSE 22/23 32/33 04 91 28 85 53 Roseline Rosas Bureau 27 r.rosas@univ-amu.fr Gaëtan Herbette Bureau 28 gaetan.herbette@univ-amu.fr L. Charles 31 20/21 C. Chendo G. Excoffier Analyse Elémentaire 30 RMN 400MHz A. Thévand 29 18/19 V. Monnier G. Herbette 28 R. Rosas 17 27 RMN 300MHz RMN 500MHz « Engineer » 25/26 15/16 Automatique RMN 600MHz RMN 400MHz

  17. NMR forms http://www.spectropole.fr

  18. Plan • Solution NMR Spectroscopy • Solution NMR Service • Solution NMR in automatic and manual mode • Contact - Form - Prices Conclusion

  19. Conclusion • Wide variety of field and probes suitable for analysis requests, allowing a very wide range of applications Liquid NMR • Non-destructive analytical technique • Possible analysis of all magnetically active nuclei • Automatic service available 24H/24, 7days/7 • Cryoprobe 600MHz higher sensitivity, ideal for structure determination for a small amount of sample

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