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Experiment 3: Preparation of an Iron Oxalate Complex Chem 105-2

Results and Discussion: After Synthesis1. In my procedure I took about 3 g of Iron (II) ammonium sulfate ((NH4)2Fe(SO4)26H2O) and dissolved it in about 25 mL of deionized water. Then I added about 25 mL of 1.0 M oxalic acid (H2C2O4) and brought my solution to a gentle boil. After this I cooled the mixture and allowed my precipitate to settle and then I decanted my precipitate twice- the first from the solution and the second after adding about 20 mL of deionized water. Next I added about 10 mL of saturated Potassium Oxalate (K2C2O2) and warmed the mixture to 40C. Then I added 30 mL of 3% hydrogen peroxide (H2O2) a few mL at a time, stirring continuously to maintain 40. Next I heated the mixture to boiling and added about 8 mL more of the oxalic acid and then 2 ML of ethanol. I placed the resulting clear green solution in a plastic cup with a lid. 2. a) The first color change reaction in the lab was between the dissolved Iron (II) ammonium sulfate in water (a clear lightly blue tinted solution) and the clear, colorless oxalic acid solutionIn this reaction the solution changed from a clear liquid with a light blue tint to a yellow liquid with the reaction forming the bright yellow precipitate. Fe(NH4)2(SO4)26H2O (aq) + H2C2O4 FeC2O4 2H2O (s) + H2SO4(aq) + (NH4)2SO4 (aq)+ 4H2O(l) The FeC2O4(s) is the yellow precipitate (Iron (II) oxalate dihydrate) we wish to decant and continue the experiment with. b) The second color change reaction was when the clear, colorless saturated Potassium Oxalate was added to the bright yellow Iron (II) oxalate precipitate. In this reaction the solution turned an opaque dark brown rust color and rust brown precipitate was produced. When the potassium oxalate is added it produces a slightly basic solution the potassium oxalate dissociates into its ions, then oxalate ions accept one hydrogen ion from a water molecule leaving one OH-. This is what results in the rust brown Iron (III) hydroxide precipitate - Fe(OH)3(s) Basically: oxidation of the ferrous ion to the ferric ion - FeC2O4 is the source of the Fe 2+ 2Fe 2+ H2O + HO2- + 2e H2O + HO2- + 2Fe 2+ 2Fe 3+ + 2e3OH2Fe3+ + 3OH(2e- "lost") (2e- "gained") (net reaction)

Thus, The OH- ion concentration of the solution is high enough so that some of the Fe3+ reacts with OH- to form ferric hydroxide (brown precipitate) as follows: Fe3+ (aq) + 3OH-(aq) Fe(OH)3(s)

Experiment 3: Preparation of an Iron Oxalate Complex Chem 105-2

c) The last reaction resulting in a color change was when the clear, colorless oxalic acid solution was added back into the mixture of the rust brown Iron (III) hydroxide precipitate and the solute Potassium Oxalate, this caused the rust brown Iron (III) hydroxide precipitate to dissolve and the mixture to turn a clear bright green- resulting in the soluble complex Potassium ferrioxalate to be formed. 3K2C2O4(aq) + 2Fe(OH)3(s) +3H2C2O4(aq) 2K3[Fe(C2O4)3] 3H2O (aq) + 3H2O(l)

3. there are many points during the process that I could have positively or negatively affected the size, quality and yield of my crystals, any of my equipment throughout the process could not have been completely clean, despite my attempts to wash with deionized water, and this would have affected my crystals, not noticeably the quality of them. When we had measured out 3 g of Iron (II) ammonium sulfate in accordance with eyeballing the sample provided by the TA it was not precise, and this would have affected my crystal results in comparison to others of my lab. I was very careful in decanting my yellow Iron (II) oxalate dehydrate, and attempted to wash it toughly so as not to cause my crystals to be of poor quality due to impurities, but despite my attempts it would be impossible to account for all previous reactants. Also, despite my attempts to measure my reactants properly, most notably my oxalic acid at the end when we used the dropper, I could have added more or less than was strictly necessary, this also would have affected the results of my crystals. Lastly, the amount of ethanol I added was different in comparison to others, and since Alcohol is added to the solution to cause the complex iron salt to precipitate this would also have affected the amount of my crystals.

After Observation-