1 / 19

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

stasia
Télécharger la présentation

SPECTROPOLE

An Image/Link below is provided (as is) to download presentation Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author. Content is provided to you AS IS for your information and personal use only. Download presentation by click this link. While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server. During download, if you can't get a presentation, the file might be deleted by the publisher.

E N D

Presentation Transcript

  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

More Related