Lab 4 and 5a report - Matthew Mueller Sept. 21, 2007 CHEM...

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Matthew Mueller Sept. 21, 2007 CHEM 207-01A SYNTHESIS AND RECRYSTALLIZATION OF Cr(acac) AND Fe(acac) Objective This lab involved the synthesis of Cr(acac) and Fe(acac) to make a crude product. It then involved the recrystallization of Cr(acac) and Fe(acac) to get a pure product. Finally it involved the determination of the melting point of the products to help determine how pure the products were. Stoichiometry Tables Cr(acac) 3 Compound Amount M.W. Moles Eqiv. Density M.P. acacH 11.8 mL 100.12 gmol .0118 mol 0.972 kgm3 -23°C Urea 19.983 g 60.07 gmol .3327 mol N/A 83°C CrCl 3 ∙6H 2 O 5.324 g 266.45 gmol .01998 mol N/A 132.7°C Fe(acac) 3 Compound Amount M.W. Moles Eqiv. Density M.P. acacH 500 μL 100.12 gmol 4.99 × - 10 6 mol 3:1 0.972 kgm3 -23°C NaC 2 H 3 COO∙6H 2 O .500 mg 136.10 gmol 3.67 × - 10 5 mol 3:1 N/A
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FeCl 3 ∙6H 2 O 0.273 g 270.3 gmol 1.01 × - 10 3 mol 1:1 N/A 37°C Synthesis of Cr(acac) 3 Procedure Observations 1. Place 100 mL of DI water in a 250 mL Erlenmeyer flask. 2. Add 5.30 g - 5.34 g of chromium (III) chloride hexahydrate (CrCl 3 ∙6H 2 O) to the flask and dissolve. Mass of CrCl 3 ∙6H 2 O = 5.324 g -CrCl 3 ∙6H 2 O dissolves into green solution 3. Add 19.8 g – 20.2 g urea ((NH 2 ) 2 CO) and 11.8 mL acacH to the flask and cover with a watch glass. Mass of Urea = 19.983 g -Urea doesn’t dissolve 4. Heat the flask by placing it in a larger beaker of boiling water (boiling chips added) for 1.5 to 2 hours till deep maroon crystals will have formed. -Separation layer in flask disappears after approx. 15 min. -Crystals start to form in approx. 40 min -Full layer of crystals formed in approx. 50 min. 5. Cool the flask to room temperature and collect the product by suction filtering. 6. Wash the crystals on the filter with several small amounts of DI water then air dry. 7. Weigh the crystals and calculate percent yield. Then place the crystals in a beaker and store in the lab station drawer. Synthesis of Fe(acac) 3
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Procedures Observations 1. Place the 10mL Erlenmeyer flask along with a magnetic stir bar onto an analytical balance and tare the weight. Mass about 270mg of Iron(III)chloride hexahydrate (FeCl 3 ∙6H 2 O) and place it into the flask. Measure 2.5mL of distilled water using a 10mL graduated cylinder and add it into the flask with the FeCl 3 ∙6H 2 O. Mass of FeCl
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This lab report was uploaded on 04/08/2008 for the course CHEM 207 taught by Professor Richardson during the Fall '08 term at University of Louisville.

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Lab 4 and 5a report - Matthew Mueller Sept. 21, 2007 CHEM...

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