90696665-Lab-Report-Final-Editied-1 - CHEMISTRY 3B:SEC 5...

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CHEMISTRY 3B:SEC 5 Laboratory Report Synthesis And Analysis Of Potassium Ferric Oxalate Akwasi Dekyi Jr. 11/27/2009 Dr. Vandana A. Bindra
Introduction This experiment involves the synthesis (combination of entities) of potassium ferric oxalate and the verification of the purity and the composition of the product derived. In this series of experiment potassium ferric oxalate will be made and analyzed. It will be analyzed in two ways. The amount of potassium ferric oxalate will be determined using a titration method. After that an independent analysis will be done by using a spectrophotometer to determine the concentration of iron in the sample. The equation for the overall reaction to obtain potassium ferric oxalate is as follows: 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) In order for potassium ferric oxalate to be produced, ferrous oxalate must be formed. The equation for the formation of ferrous oxalate is given as follows: Fe(NH 4 ) 2 .SO 4 .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) .3H 2 O (s) Before we determined the concentration of iron in our sample, the iron in our product was made into a new complex using phenanthroline molecule. Then iron was reduced by the compound hydroxylamine hydrochloride. The equation for the formation of the complex iron (ii) and the reduction of iron (iii) by hydroxylamine is as follows: Fe +2 + 3C 12 H 8 N 2 Fe(C 12 H 8 N 2 ) 3 +2 (Formation of Fe +2 ) 4Fe +3 + 2H 2 NOH 4Fe +2 + N 2 O + 4H + + H 2 O (Reduction of Fe +3 ) The amount of oxalate ion in the sample was then determined by titrating the solution of the product with potassium permanganate. The equation is given as follows; 5C 2 O 4 -2 + 2MnO 4 - + 16H + 10CO 2 + 2Mn +2 + 8H 2 O Method The instruments used for 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 aqueous solution, burette for titration, thermometer for temperature readings, pipette for transferring the liquid, volumetric flasks and test tubes . The synthesis of the co-ordination compound, potassium ferric oxalate trihydrate was done by firstly by the preparing ferric oxalate. This was done by adding a sufficient amount of Fe (NH 4 ) 2 (SO 4 ) 2 .6H 2 O with H 2 SO 4 and oxalic acid which in this experiment was 5grams. The solution
was clamped to a ring stand and using a Bunsen burner the solution was heated to allow the reaction to occur. A yellow solid then appeared when the reaction occurred, this solid was FeC2O4.2H2O. The yellow liquid was then poured and the flask was again placed on the ring stand and 20ml of deionized water was added to the solid and was heated again. The solution was heated again get rid of the ammonium bisulfate tetra hydrate (2(NH4)HSO4 + 4H2O).This was then mixed

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