Experiment 8

Experiment 8 - Heather McMillen 2.3.9 December 3 2007...

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2.3.9 Heather McMillen December 3, 2007 Experiment 8: Preparation and Analysis of an Iron Salt Introduction: In this lab, the purity and percent yield of a compound, potassium tris ferrate trihydrate salt, was measured. These values were used to determine whether or not this experiment would be useful for a pharmaceutical company that is looking to produce generic drugs. The purity was determined by calculating the percent oxalate, percent iron (III), and percent of potassium in the compounds. The percent yield was calculated using the theoretical yield. Experimental: First, the salt needs to be prepared. In a 250 mL beaker, 7.5 g (Fe(NH4)2(SO4)2 * 6H2O was weighed out using an analytical balance and dissolved in 25 mL of 1mL of 6M sulfuric acid mixed with warm water. 35 mL of oxalic acid solution (C2O4-2/Fe2+ = 1.5) was stirred in the solution and heated to the point of steaming. Once the granular yellow precipitate of ferrous oxalate settled, the clear liquid was poured out. The oxalate was stirred with 25 mL of hot water and the clear wash water was poured out. 15 mL of prepared 1.8 M potassium oxalate solution was added to the solid and warmed to 40 degrees Celsius. Ferric hydroxide was formed and then dissolved by heating the mixture to boiling, adding 8 mL of oxalic acid solution, then adding a small portion of oxalic acid until precipitate dissolves. 50 mL of green solution remained. The solution was then acquired by using vacuum filtration. The crystals were washed three times with 5 mL of 1:1 water-ethanol mixture, twice with 5 mL of acetone, and dried by vacuum filtration. 1
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2.3.9 Heather McMillen December 3, 2007 For the oxalate analysis, a 50 mL burette was cleaned and rinsed with DI water and then rinsed with two 5 mL portions of 0.1000 N KMnO4 and filled with 0.1000 N KMnO4. 0.10XX g of the prepared salt was dissolved in 20 mL 6 M sulfuric acid and was heated to boiling. The hot solution was titrated with 0.1000 N KMnO4. This titration was repeated again: trial 2. For the K
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This note was uploaded on 04/07/2008 for the course CHEM 104a taught by Professor Mcmillen during the Fall '07 term at Vanderbilt.

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Experiment 8 - Heather McMillen 2.3.9 December 3 2007...

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