IIIIV V V V ANALYSE RMN ANALYSE RMN ANALYSE RMN ANALYSE RMN
A. RMN 1 H (1D) température de la sonde : 25° C.
- largeur spectrale: 10000 Hz. - taille du FID: 32K. - taille du spectre: 64K. - durée de l’impulsion: 8 µs. - angle de basculement : ≈90°. - délai entre les impulsions: 3 s.
- temps d’acquisition : 4.6 s. - nombre d’accumulations: 128. E. RMN 2D (DOSY)
- séquence utilisée pour les formulations solides : Echo de spin stimulé avec gradients bipolaires (stebpgp1s). Une séquence d’impulsion 3-9-19 avec des gradients de 9.25 G.cm-1 a été ajoutée pour la suppression du signal de l'eau pour les formulations liquides de FLX.
- température de la sonde : 25° pour les formulations solides et 32° pour les formulations liquides.
- largeur spectrale: 10000 Hz (F2) - taille du FID: 32768 (F2) * 40 (F1). - taille du spectre: 2048 (F2)
- délai entre les impulsions: 2 s. - nombre d’accumulations: 64.
- durée de l’impulsion 90° P1 : 8.25 µs.
- durée de l’impulsion P2 : 16.50 µs
- délai de diffusion D20 (∆) : 0.08-0.12 s.
- durée du gradient P30 ou δ/2 : 1000-1700 µs.
Partie Expérimentale du Chapitre 2.
- étendue du gradient : 5 % à 95 %. - nombre de points (expériences) : 40.
-échantillonnage du gradient : linéaire.
-intensité maximale du gradient : 46.25 G.cm-1.
Les paramètres de la séquence ont été adaptés afin d'avoir l'intensité du signal de FLX (H4,6)
ou de FLV (H3,4,6,7) fortement diminuée (au moins divisée par 50) à 95% de l’intensité maximale
du gradient. Les données spectrales sont traitées avec le logiciel de RMN Gifa5© commercialisé
par la société NMRtec (Montpellier, France). Ce logiciel propose un module spécifique de traitement des expériences DOSY basé sur la transformée inverse de Laplace.
- nombre de points : 2048. - itération MaxEnt : 20 000. - nombre de colonnes : 32.
Bibliographie du Chapitre 2.
Bibliographie
Bibliographie
Bibliographie
Bibliographie
Bibliographie du Chapitre 2.
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