Nifedipine bildet in unterkiihlten Schmelzen zwei neue Modifikationen: Eine bei 162O-164O schmelzende Modifikation I1 (feinstrahlige Aggregate) sowie eine weitere polymorphe Modifikation I11 (balkenformiger Kristallhabitus), die zwischen 134O-137O schmilzt.
The spatial structure of gels of sodium carboxymethyl cellulose (NaCMC-gel) and carboxymethyl cellulose in the free acid form can be imaged in the transmission electron microscope (TEM). The freeze-fracturing technique is suitable for this. Experiments with test preparations (10 % aqueous glycerol solution) show that cooling rates during freeze-fixing are decisive for visualization, and that cooling rates can be improved substantially by using a cryojet. The increase of the cooling rate to more than 15 000 K/s makes it possible to obtain extremely fine network structures with a mesh width of 5-25 nm and with a filament thickness of 2-3 nm. The results obtained after jet-freezing show differences in the structure of the two gels: quasi-crystalline microaggregates in the HCMC-gel can be seen, and they cause an increased elasticity and opalescence of the aged HCMC-gels.
26 6,7-Diacetyl-teloidin-3-benzhydrylitther (XXXV):Eine h u n g von 1,29 g IV') (6 mMol) und Diphenyldiammethe, bereitet aue 3,92 g (20 mMol) Benzophenonhydrazon und 4,4 g (20 mMol) Quecksilberoxyda'), in 10 ccm absol. Benzol wurde 24 Stunden am RiickfluB gekocht. Die Reaktioneltisung wurde mit Benzol verdiinnt, mehrfach mit 2x1 HCl auegachiittelt und die salzsaure Phase nach einmagem Durchachiitteln mit hither mit 30%iger Natrodauge alkaliech gemacht. Daa abgachiedene 01 wurde mit &her aufgenommen, der nach dem Trocknen und Abdatillieren des hithers verbleibende Ruckstand kristallisierte rmch durch; 1,74 g (80% d. Th.) vom Schmp. 136'. XXXV wurde aus Petrolather (60/76') in farblosen Nadeln vom Schmp. 142-144" erhslten. C,,Hz&O, (423.6)Ber.:
Aqueous gels of carboxymethylcellulose in the free acid form (HCMC) are obtained when dialyzed sodium carboxymethylcellulose (NaCMC)-gels are treated with a strongly acidic ion exchanger. These gels age rheologically. During the aging process (maximum 60 days), thixotropy and increased viscoelasticity occur. The rheological changes are measured by shear viscosity r/, coefficient ofthixotropy H, complex dynamic shear modulus G*, shear storage modulus G', shear loss modulus G", and tangent of the phase angle. The aging process is caused by the formation of quasi-crystalline microaggregates of HCMC which can be detected by electron microscopy (Part II).
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