The use of gel permeation chromatography ( G P C ) for the characterization of unsaturated polyester resins is demonstrated on several examples. Number-average molecular weights determined by this method are compared to data obtained by means of vapor pressure osmometry ( V P O ) and by end group analysis ( E G ) . The determination of t h e polyester resin composition as a function of molecular weight by stop-and-go UV scanning procedure is described.
ZUSAMMENFASSUNG:Phenol-Formaldehyd-Harze vom Novolak-und Resol-Typ wurden durch Chromatographie an einer mit Octadecylsilan auf Kieselgel bepackten Umkehrphasen-Mikro-Saule getrennt. Eine gute Auftrennung der meisten Komponenten wurde durch die Verwendung der Gradientelution mit Methanol und Wasser erzielt . Der Gradient wurde in einer Rohr-Mischkammer (Volumen 1 3 ml) erzeugt; der Anteil von Methanol in der mobilen Phase wurde im Verlauf der Analyse von 10 auf 90% kontinuierlich gesteigert. Die Probenaufgabe erfolgte mit Hilfe eines Dosierventils und einer Probenschleife (Volumen 10 pl). Das Verfahren ergab reproduzierbare Ergebnisse; es erwies sich als gut geeignet zur Charakterisierung von Phenol-Formaldehyd-Harzen.
A liquid chromatographic method for the determination of flucytosine in capsules was collaboratively studied by 7 laboratories. The method uses a C18 reverse phase column, water-methanol-acetic acid mobile phase containing 1-octanesulfonic acid sodium salt, p-aminobenzoic acid as internal standard, and photometric detection at 285 nm. The mean recovery value (±SD) of flucytosine from a synthetic formulation representing capsules was 99.2 ± 1.72% (CV = 1.73%). Composited samples of 250 and 500 mg commercial capsules gave assay values of (mean ± SD) 103.17 ± 2.21 and 99.29 ± 1.29% of declared, respectively. CV values were 2.15 and 1.30%. Reproducibility and repeatability CVs were 2.19 and 1.50%, respectively, for the 250 mg capsules, and 1.34 and 0.63%, respectively, for the 500 mg capsules. The method has been adopted official first action.
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