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Synthesis and Analysis of Potassium FerricOxalate Gia Caroluzzi11/9/2017Professor ChabraChemistry 003B 011 of 13
Introduction This experiment involves the synthesis of potassium ferric oxalate and the verification of the purity and the composition of the product derived. In this series of experiments potassium ferric oxalate will be composed and analyzed. Using a titration method, the amount of potassium ferric oxalate will be determined. Then analysis will be done using a spectrometer to determine the concentration of iron in the sample. The equation for the overall reaction to obtain potassium ferric oxalate is:2FeC2O4. 2H2O(s) + H2O2(aq) + H2C2O4(aq) + 3K2C2O4(aq)2K3Fe(C2O4)3. 3H2O(s)Ferrous oxalate must be formed, in order for potassium ferric oxalate to be produced. The equation for the formation of ferrous oxalate is: Fe(NH4)2(SO4)2. 6H2O(aq) + H2C2O4(aq)FeC2O4. 2H2O(s) + 2(NH4)HSO4(aq) + 4H2O Before the concentration of iron in the sample can be determined, the iron in the product is transformed into a new complex using the phenanthroline molecule. Then iron is reduced by the hydroxylamine hydrochloride compound. The equation for the formation of the complex of iron(ii) with phenanthroline is as follows: Fe+2+ 3C12H8N2Fe(C12H8N2)3+2 The equation for the reduction of iron(iii) by hydroxylamine is as follows: 4Fe+3 + 2H2NOH4Fe+2+ N2O + 4H+ + H2OThe amount of oxalate ion in the product will be determined by titrating the solution of the product with potassium permanganate. This equation is as follows: 5C2O4-2+ 2MnO4- + 16H+10CO2(g) + 2Mn+2 + 8H2O 2 of 13
Method The instruments used in this experiment were; beakers to contain the samples, Bunsen burner for the conversion of compounds, a spectrophotometer to read the absorbance and transmittance of complex solutions, filter paper for the separation of the solid from the aqueoussolution, burette for titration, thermometer for temperature readings, pipette for transferring the liquid, volumetric flasks and test tubes. The synthesis of potassium ferric oxalate trihydrate was done by firstly by preparing ferric oxalate. This was done by dissolving 5 grams of Fe(NH4)2(SO4)2.6H2O with 15 ml of deionized H2O and 5 drops of 3M H2SO4. This was then combined with 25 ml of a 1M oxalic acid solution, producing a yellow solution. The solution was clamped to a ring stand and using a Bunsen burner the solution was heated to allow the reaction to occur. Once the reaction has occurred a yellow solid appears. The yellow liquid was then poured and the flask again placed on the ring stand and 20 ml of deionized water was added to the solid and was heated again. The solution was heated again to get rid of the ammonium bisulfate tetra hydrate. The liquid was then decanted from the solid, this solid is FeC2O4.2H2O. 10 ml of saturated Potassium oxalate was then added to the solid, producing a dark orange solution. A solution of 20 ml of 3%H2O2was placed into a beaker while 8 ml of 1M H2C3O4was placed into a graduated cylinder.