The experiment was conducted, which metals manganese (Mn3+), Cobalt (Co3+) and Copper Cu3+ was prepared and acac complexes where also obtained. Recrystallization was performed of which Mn(acac)3 ,Co(acac)3 and Cu(acac)3 was obtained at percentage yield of 32%, 85.6% & 92% for each of acac’s. TLC was performed which results deduced unknown mixture both contained manganese and cobalt since it had the same Rf vaues.
Experiment aims
The aim of the experiment was to prepare metal acetylacetonate complexes and also characterization by studying the (Thin Layer Chromatography (TLC) and reading IR spectra of the acetylacetonate complexes).
Results and Discussion
Table 1: The character and mass of Mnacac3. Compound | Mass Obtained/g | Colour of Crystals | Melting Points | | | | Literature Value | Measured Value | Mnacac3 | 0.989 | Strong Brown | 160 °C | 150-159.5°C |
Synthesis of Mn3+ Complex
The reaction mixture of 1.3 g of MnCl2.4H2O and 3.4g of sodium acetate in 50cm3 of distilled water. Then 5 g of acetyl acetone allow shake then addition of 0.29 g of KMnO4 in 12.5cm3 of distilled water. A strong black of 2.19 g products was obtained then brown acac after recrystallization was obtained. The equation below simply explains the reaction:
5Mn2++MnO4-+15(CH3CoCH2COCH3)3→2H2O+7H++5Mn(CH3COCHCOCH3)3
Moles for Mn(acac)3: 0.00904mol
MW of MnCl2.4H2O: 143.856 gmol Mass ofMnCl2.4H2O: 1.3 g
Moles of acetyl acetone: 0.0499 mol
Manganese (II) chloride tetra hydrate and acetyl acetone reacts in a 1:1 stoichiometric ratios and therefore Manganese (II) chloride tetra hydrate is clearly a limiting reagent for the reaction above. The maximum amount of Manganese (II) chloride tetra hydrate that can be formed is 0.00904 mol.
Mass of
Mnacac3 (g) = number of moles × Molecular Weight = 9.04×10-3mol ×352.258gmol = 3.18g
Percentage Yield = actual amount of producttheoretical amount of product ×100
References: 1. Wekipedia, 2013, Accessed 23 April 2013 [Internet] http://en.wikipedia.org/wiki/Moolooite Infrared_spectroscopy. 2. LAMPREY, H. (1960) Properties and Applications of metal acetylacetone.. Vol. 18, No. 11, 359-400.