Component analysis and purification of industrial grade n-octylferrocene

The components of industrial grade n-octylferrocene were analyzed by gas chromatography-mass spectrometry(GC-MS), and the purity of n-octylferrocence is only 90.00%. The main impurities are some homologs and isomers of ferrocene. With the relative content and recovery of product as index of purification, several methods were utilized to separate and purify n-octylferrocene, such as vacuum distillation, column chromatography, and recrystallization. The results show that the most effective method is recrystallization under a mixed solvent after several times at low temperature. The recrystallization condition: crystallization solvent, blended solvent ratio, crystallization temperature and time, as well as times of crystallization were investigated in detail. The results show that the higher purity of n-octylferrocene can be obtained under blended solvent ratio(ethyl acetate: methanol: hexane=2∶2∶5(volume)), along with 6 times recrystallization at minus 50℃. The final purity is determined by gas chromatography(GC) and H-nuclear magnetic resonance(¹HNMR), which is over 99.50%, and the recovery is 73.0%.