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. Dans-un-ballon, 84 g (0,01 mol) de K 4 W(CN) 8 ?2H 2 O, 1,38 g (0,02 mol) de nitrite de sodium NaNO 2 dans 100 ml d'eau. Mettre sous agitation. A l'aide d'une ampoule à brome, y ajouter en goutte à goutte 5

. Dans-un-bécher, 6 mmol) de {(C 4 H 9 ) 3 NH} 3 [W(CN) 8 ]?4H 2 O dans un minimum de méthanol (environ 5 ml) Dissoudre séparément trois équivalents de chlorure de césium CsCl dans un minimum de méthanol, préalablement chauffé à 50°C Compléter la dissolution en ajoutant quelques gouttes d'eau. Mettre sous agitation, puis ajouter la solution chaude de chlorure de césium à celle du complexe octacyanométallate. Il se forme instantanément un précipité jaune, Cs 3 [W(CN) 8 ]?2H 2 O. Le filtrer sur un fritté de porosité 4

. Dans-un-bécher, CoCl 2 ?6H 2 O, 165 mg (1,6 mmol) de 3- CNpy dans 8 ml d'eau. Mettre sous agitation. La solution est de couleur rose. Dans un deuxième bécher, protégé de la lumière par du papier d'aluminium, dissoudre 700 mg (0,85 mmol) de Cs 3 [W(CN) 8 ]?2H 2 O dans 8 ml d'eau. Mettre sous agitation. La solution est d'une MESURES OPTIQUES Les mesures optiques ont été effectuées à l'ICMCB sur des appareillages de réflectivité

. Durant-les-mesures, échantillon est irradié en permanence et la lumière réfléchie est récoltée par un photomultiplicateur. Les appareils sont calibrés en enregistrant les spectres de réflectivité du noir de charbon comme standard noir (réflectivité = 0 %) et du sulfate de baryum comme standard blanc (réflectivité = 100 %) Deux appareillages à liquide cryogénique azote

L. Réflectivité-hélium, un spectromètre type CVI, d'une lampe Oriel, 9V délivrant une puissance de 90 mW.cm -2 en surface de l'échantillon. Le porte-échantillon est placé au bout d'une canne, contrôlée de manière automatique par le logiciel, et introduit directement dans la bouteille d'hélium. La régulation de la température s'effectue en ajustant la hauteur de l

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