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Synthesis and Analysis of K 3 Fe(C 2 O 4 ) 3 •3H 2 O
Introduction There are two purposes of this experiment; the first is to synthesize potassium ferric oxalate. After the synthesis of K 3 Fe(C 2 O 4 ) 3 •3H 2 O is done, the second purpose is to analyze in order to determine the purity of what we made. In order to figure out the purity of our product, we need to find the percent iron and percent oxalate found. The first step is to produce ferrous oxalate (FeC 2 O 4 2H 2 O), which is a yellow insoluble solid. All the other reactants and products used in the reaction to produce ferrous oxalate are soluble. Fe(NH 4 ) 2 (SO 4 ) 2 6H 2 O (aq) + H 2 C 2 O 4 (aq) FeC 2 O 4 2H 2 O (s) + 2(NH 4 )HSO 4 (aq) + 4H 2 O The second step is to produce potassium ferric oxalate, a green solid. This will be produced by oxidizing the ferrous oxalate by hydrogen peroxide in the presence of oxalate ion. 2FeC 2 O 4 2H 2 O (s) + H 2 O 2 (aq) + H 2 C 2 O 4 (aq) + 3K 2 C 2 O 4 (aq) 2K 3 Fe(C 2 O 4 ) 3 3H 2 O (s) Then the product is analyzed through two methods. First, the potassium ferric oxalate will be titrated with a solution of potassium permanganate to determine the amount of oxalate ion present. The permanganate ion will only react with the oxalate ion present. 5C 2 O 4 -2 + 2MnO 4 -2 + 16H + 10CO 2 (g) + 2Mn +2 + 8H 2 O The second method is finding the concentration of iron in our sample using a spectrophotometer. Iron then undergoes reduction using the hydroxylamine hydrochloride compound. 4Fe +3 + 2H 2 NOH 4Fe +2 + N 2 O + 4H + +H 2 O
Experimental Part 1, Synthesis of an Iron Compound: Fe(NH 4 ) 2 (SO 4 ) 2 6H 2 O (5.05 g) was added to 15 ml of deionized water in an Erlenmeyer flask. 5 drops of 3M H 2 SO 4 was then added. After the solid was dissolved, 25 ml of 1M oxalic acid solution was added. The solution was then heated to a boil, followed by letting the solid settle. After, the liquid was poured into a beaker, leaving the yellow solid behind. 20 ml of deionized water was added to the yellow solid and was then heated. The solid settled and the liquid was decanted, leaving behind FeC 2 O 4 2H 2 O. 10 ml of a saturated potassium oxalate was added to the solid, and then heated to 40 . When 40 was reached, 20ml of H 2 O 2 was added slowly with constant stirring, and then heated to a boil. About 5 ml of 1M H 2 C 2 O 4 solution was added to the boiling solution, followed by mixing, and then a filtration. When the solution was cooled, it was transferred into a beaker and then 10 ml of ethyl alcohol was added. The beaker was then placed in the drawer after being covered with a piece of filter paper. During the next lab period the solid was collected by a simple filtration. The crystals were washed with a solution of 5 ml of ethyl alcohol and 5 ml deionized water, and then were blotted dry. The weight of the product was then obtained yielding 1.7 g.

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