Limites et Potentiel de la RMN pour la caractérisation structurale de l environnement des éléments «traces»
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1 Limites et Potentiel de la RMN pour la caractérisation structurale de l environnement des éléments «traces» USTV - REACH Thibault Charpentier 25 Novembre septembre 2013 CEA 10 AVRIL 2012 PAGE 1
2 NMR of Glasses Solid State Nuclear Magnetic Resonance (ssnmr) is a powerful spectroscopy to probe the glass structure at the atomic scale. N. Ollier CEA/DSM S. Peuget CEA/DEN F. Angeli P. Jollivet CEA/DEN S. Schuller CEA/DEN Composition Structure Properties Thibault Charpentier - USTV REACH Novembre 2013 PAGE 2
3 Basic Principles of NMR 23 septembre 2013 PAGE 3
4 NMR : the polarization NMR : low frequency ( MHz)
5 NMR and the periodic table
6 RMN pulsée B 0 Sample B RF Excitation Detection Coil
7 NMR interactions and the local atomic environment (1) Main NMR parameters : (2) Only for I>1/2 Quadrupolar Interaction speciation / structural units Connectivities Proximities (2D) Isotropic chemical shift (position of the line) (1) δ iso Quadrupolar coupling constant (width of the line) (2) Asymmetry parameter (lineshape ) C Q η
8 NMR : Liquid versus Solid Rigid lattice (powder) NH2-CH2-COOH Tissues -Food Brownian Motion Narrow lines Peak Aera = Quantification Thibault Charpentier - USTV REACH Novembre 2013 PAGE 8
9 RMN : Une spectroscopie non-destructive Using NMR to study full intact Wine bottles, A.J. Weekley et al., JMR 161 (2003) C NMR, 2.01 T scans Detection of cocaine (1min, 5mM 1.5g/L)! (Gambarota et al. 2011) Drug testing and Analysis 3 (2011) 544
10 Magic Angle Sample Spinning (MAS) NMR Static Low MAS * : Spinning sidebands MAS Thibault Charpentier - USTV REACH Novembre 2013
11 MAS NMR of 29 Si in binary Na 2 O-SiO 2 glasses (1) (1) Chemical disorder (2) (2) Geometrical disorder Geochimica et Cosmochimica Acta 75 (2011) 2453 PAGE 11
12 Advanced NMR techniques : two spin interactions Double-Quantum (DQ) MAS NMR Probing spin pairs Through chemical bonds 23 septembre 2013 Coll. S. Schuller, F. Angeli, CEA/DEN PAGE 12
13 RMN MAS : résolution de la structure des verres à l échelle moléculaire Thibault Charpentier - USTV REACH Novembre 2013 PAGE 13
14 MAS NMR of Quadrupolar Nuclei (I>1/2) MAS removes only partially Second Order Quadrupolar (SOQ) Broadening Central Transition (-1/2) (+1/2) Multiple-Quantum MAS (2D) removes SOQ anisotropy Q (2) 1/ν O PAGE 14
15 11 B MAS NMR in borosilicate glasses 1-10%mol Texp~min Detection level ~ ppm See F. Angeli et al., JACerS 93 (2010) Thibault Charpentier - USTV REACH Novembre septembre 2013 PAGE 15
16 RMN : Importance de la spéciation des traces Thibault Charpentier - USTV REACH Novembre 2013 PAGE 16
17 RMN : Importance de la spéciation des traces 11 B MAS NMR, 16.4 T scans Thibault Charpentier - USTV REACH Novembre 2013 PAGE 17
18 RMN : spéciation de traces Spéciation du bore = mesure du ph de l océan (µmol/kg) Thibault Charpentier - USTV REACH Novembre 2013 PAGE 18
19 RMN : spéciation de traces 18.8 T 11 B MAS NMR, 20 khz 40-50h (1s* ) 9.4 T Thibault Charpentier - USTV REACH Novembre 2013 PAGE 19
20 17 O MAS & MQMAS NMR See F. Angeli et al., JNCS 354 (2008) Thibault Charpentier - USTV REACH Novembre 2013
21 Application to MoO 3 ( in low concentation) incorporation in silicates Angeli 23 septembre et al. GCA PAGE 21
22 Help of DFT to identify NMR fingerprint 23 septembre 2013 PAGE 22
23 95Mo MAS NMR 5%mol MoO3 2%mol MoO3 2%mol MoO T (500WB) Texp ~ 1-2 days 23 septembre 2013 Thibault Charpentier - USTV REACH Novembre 2013 PAGE 23
24 17O NMR : indirect detection of heavy element? 60SiO 2 35Na 2 O 5La 2 O 3 B 0 =11.7 T B 0 =7.1 T La contribution La contribution ~1-0.1%mol La2O3 can be resolved if resolution is achieved (and fingerprint known) Separation between Si-O-Na/Si-O-Si is enhanced at lower magnetic field (-> enables to refine the quantifications) Thibault Charpentier - USTV REACH Novembre 2013 PAGE 24
25 17O MAS / MQMAS NMR B 0 =11.7 T B 0 =7.1 T [4] 2( Na2O B * B2O3 xna La2O3 ) Si O Na = O 2(3La2O3 + xna La2O3 ) Si O ( Na, La) = O Agreement with experiment considering La-Na mixing: 3.3 Na + for 1 La 3+ La-Na mixing: 6.3 positive charge - requires the same NBOs - La coordination ~ 6 F. Angeli et al., JNCS (2013) Thibault Charpentier - USTV REACH Novembre 2013 PAGE 25
26 RMN de métaux lourd dans des verres Texte 207Pb NMR 29Si NMR Thibault Charpentier - USTV REACH Novembre 2013 PAGE 26
27 RMN des métaux lourds en solution (RMN liquide) Thibault Charpentier - USTV REACH Novembre 2013 PAGE 27
28 NMR Sensitivity is (still) an issue! Sample Coil Detection Filling factor + Higher Resolution : higher sensitivity NMR peak aera is proportional to the number of spins (Quantitativity) NMR sensitivity = Polarisation x Detection x Resolution
29 Low temperature MAS-NMR 25K 40K 79K Thibault Charpentier - USTV REACH Novembre 2013 PAGE 29
30 RMN MAS : CryoMAS Thibault Charpentier - USTV REACH Novembre 2013 PAGE 30
31 HR-MACS-NMR : RMN miniaturisée (A. Wong, D. Sakellariou, LSDRM) Thibault Charpentier - USTV REACH Novembre 2013 PAGE 31 Thibault Charpentier - USTV REACH Novembre 2013
32 DNP MAS NMR : use high frequency polarization High frequency Coupling Thibault Charpentier - USTV REACH Novembre 2013 PAGE 32
33 RMN MAS : DNP et surface Thibault Charpentier - USTV REACH Novembre 2013 PAGE 33
34 RMN MAS : DNP et surface Thibault Charpentier - USTV REACH Novembre 2013 PAGE 34
35 RMN MAS : Dynamic Nuclear Polarization - DNP (Hyperpolarisation)!!! Nat. Abund. 17O excited near or on the surface!!! Thibault Charpentier - USTV REACH Novembre 2013 PAGE 35
36 129 Xe NMR : Hyperpolarization (LSDRM) 1 Optical Pumping 2 Angular momenta of photons 1 Electron spins of 2 an alkali-metal Nuclear spins of a noble gas Lifetime of Xenon polarization ~hours!! Thibault Charpentier - USTV REACH Novembre 2013 PAGE 36
37 129 Xe NMR: detecting trace elements in solution (LSDRM) Cryptophan e Spacer NTA (d) (c) Specific chemical shift effect to Zn 2+ (Pb 2+, Cd 2+, ) (b) Towards nm detection! (one-scan) (a) P. Berthault et al., LSDRM Thibault Charpentier - USTV REACH Novembre 2013 PAGE 37
38 Conclusion NMR provides valuable information on chemical environment in crystalline and amorphous materials (High-Resolution) (and in solution) Standard Sensitivity mg. 0.1 (-0.01%mol) ( 0.1%weight 27 Al ) 27 Al, 11 B, 7 Li, 31 P, 23 Na mol (but background signal) 113 Cd (I=1/2), 207 Pb (I=1/2), 205 Tl (I=1/2), 199 Hg (I=1/2)? (~1 days) NMR sensitivity is «still» an issue by Hyper-NMR is coming (x100) Hyper-Polarisation (DNP, Xenon, Parahydrogen, ) Hyper-Dectection (Optical detection, ) Effective Methodologies for surface studies now exists! Sensitive (indirect) probe of trace elements exist with Hyper Resolution ( 129 Xe) NMR is also a tool for Food profiling ( 1 H, 13 C, 23 Na) Thibault Charpentier - USTV REACH Novembre 2013
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