Separation of Ferrocene and Acetylferrocene by Chromatography

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Separation of Ferrocene and Acetylferrocene by Chromatography

By | March 2007
Page 1 of 6
Purpose

1.To prepare a dry-packed sample of product mixture of ferrocene and Acetylferrocene 2.To separate and purify the components in the product mixture by column chromatography. 3.To check the purity of the components by thin-layer chromatography (TLC). 4.To calculate the yield of acetylferrocene and the percent recovery of unreacted ferrocene.

Table of Quantity showing various physical properties
Type of substanceMolecular FormulaMolecular Weight (g/mol)Density(g/cm3)M.P.(oC)B.P.(oC)Solubility FerroceneC10H10Fe186.031.49172 oC-174 oC249oCInsoluble in water, soluble in organic solvent Acetyl-ferroceneC12H12FeO228.08-81 oC -83 oC161 oC - 163 oC (at 4 mm)Very slightly soluble in water, soluble in organic solvent Ethyl AcetateC4H8O288.110.897-83.6 oC77.1 oCSlightly soluble in water (~8.3g/100mL, 20 oC), very miscible with alcohol, ether, acetone, benzene. HexaneC6H1486.180.6548-95 oC69oCImmiscible with water

Dichloro-methaneCH2Cl284.93-97 oC40 oC1.325Slightly soluble in water (~1.3g/100mL, 20 oC), very miscible with most organic solvent.

Hazard
1.Ferrocene is highly flammable and it is harmful if swallowed. 2.Acetylferrocene is highly toxic if swallowed.
3.Ethyl acetate is irritant and flammable.
4.Dichloromethane is a suspected carcinogen.
Procedure
1.The mass of the product mixture was measured.
2.About 2mL of CH2Cl2 was added to the product mixture in a 30mL beaker and about 300mg of silica gel was added 3.The beaker was covered with aluminum foil with a hole and was CH2Cl2 was evaporated. 4.2.3g of fresh silica gel was mixed with 7mL of hexane in a 30mL beaker to get a slurry. 5.Stirred the slurry constantly with hexane added and poured it into the column. 6.Hexane was added and run until the solvent was about 1cm above the silica gel. 7.About 1cm of sand was added followed by loading of the dried sample. 8.Hexane was added and run until the first fraction was collected in a 10mL...
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