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13. (2 weeks) (LSM) Metal Acetyl-acetonate Complex Purpose The purpose of this two-week lab in week one is to prepare an Acetyl-acetonate complex and be familiar with inorganic synthesis technology. Then, in the following week we are determining the melting point of the recrystallized product. Introduction In part 1 of this experiment, iron(acac)
3
is being synthesized due to the binding of acetyl-acetonate, with an iron ion to form the octahedral structure. Metal ions can bind with neutral molecules or anions, called ligands to form a coordination complex. The ligand in this case acts as a Lewis base and forms a bond with the metal ion (the Lewis acid). The next part involved the recrystallization of the product which is done to put the product in its purest form. In this experiment the acetylacetonate ion will coordinate with the iron (III) to form the octahedral Fe(acac)
3
complex. Procedure Synthesis of Fe(acac)
3
Please refer to pages 175-179 of First-Year Laboratory Manual: Chemistry 112.
1
Recrystallization of Fe(acac)
3 Please refer to pages 180-183 of First-Year Laboratory Manual: Chemistry 112.
1
Observations Part 1: The powder (FeCl . 6H2O) is a pale yellow, as is the colour of the solution. The liquid form of acetylacetone is colourless. Using a Pasteur pipette, acetylacetone is added to the FeCl.6H2O solution; the solution turns a brown, red colour. The powder form of the sodium acetate is white, while the solution is colourless. Once all content is added, the whole product is red and once filtered, the powder is also red. Part 2: The dark red solution is obtained by adding heated methanol to the crude product. Methanol is evaporated by the dark red in the hot bath, causing little crystals to develop on the bottom of the beaker. When the methanol is evaporated, a dark crimson powder will show up. The filter paper displays the dark red powder after crystallization. The product melted within 5 minutes in the machine. DATA SHEET Crude Fe(acac)
3
Experimental Observations: [These should be written directly into your lab notebook.] Mass of FeCl
3
∙6H
2
O /g: 1.00g Mass of watch glass /g: 29.46g Mass of watch glass and crude product /g: 31.552g
(before recrystallization) Recrystallized Fe(acac)
3 Mass of watch glass /g: 34.973g Mass of watch glass and pure product /g 35.973g
(after recrystallization) Calculations
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