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Synthesis and analysis Potassium Ferric Oxalate Trihydrate K3Fe(C2O4)3•3H2OAbstract Potassium ferric oxide, first step was synthesizing by combining hot ferric oxalate dihydride with potassium oxalate, hydrogen peroxide and oxalic acid. Next, we let the solution of K3Fe(C2O4)383H2O with ethyl alcohol sit for a week to grow green crystals. The experiment produced 60.9% of the theoretical yield and, there was a 34.56% error in the analysis of iron inK3Fe(C2O4)3•3H2O.The oxalate analysis showed a 19.25% error in the percent of oxalate by mass. the experiment overall showed a very high margin of error , it out of the expected 5% margin of error in the molecular formula for potassium ferric oxalate trihydrate. Hannah Kloeber November 30, 2018 CHEM 003B-QR8 Dr.I.Katash
Introduction The purpose of this experiment was to synthesize Potassium Ferric Oxalate, K3Fe(C2O4)3·3H2O, then comparing the solution made in lab to a standardized version, then analyzing the sample in a spectrometer and finally a oxidation-reduction titration. The first part of the three-week lab was the formation of ferric oxalate FeC2O4·2H2O. This was achieved by adding iron ammonium sulfate and a solution of oxalic acid and water, Fe(NH4)2(SO4)2(s)+6H2O(l)+H2C2O4(aq). The next part was creating solid potassium ferric oxalate solution with water, 2FeC2O4·2H2O(s)+H2O2(aq)+H2C2O4(aq)+3K2C2O4(aq) →2K3Fe(C2O4)3·3H2O(s). This was done by combining a oxalic acid and potassium oxalate with hot ferric oxalate. The next week crystals had formed after the week of rest. The next step was collecting the crystals by filtering them through filer paper and then drying with blotting paper. After the crystals were collected, they were put into a flask to combine with hydrogen sulfate and then diluted with DI water to form a solution. Next part of the solution was separated in a different flask and diluted, solution B. The first part of the solution, solution A, was also diluted then left to be used for analysis in a later part of the lab. Then solution B was mixed with hydroxylamine hydrochloride ,4Fe3++2H2NOH →4Fe2++N2O+4H++H2O so that it would reduce the iron. After that phenanthroline and sodium acetate were added to create an iron complex, Fe2++3C12H8N2→Fe(C12H8N2)32+, it was then analyzed in a spectrophotometer to determine its concentration in relation to the solutions with known concentrations. Solution A was stored until the final week of the lab and titrated in a redox reaction with standardized potassium permanganate, 5C2O42-+2MnO4-+16H+ →10CO2+2Mn2++8H2O, to determine the amount of oxalate ions in the solution. Experimental Weigh 5 grams of solid Fe(NH4)2·6H2O, then put it into a 250mL Erlenmeyer flask that has 15mL of DI water in it swirl to dissolve. Add 5 drops 3M H2SO4 swirl again. make sure all solid has dissolved then, add 25mL of 1M oxalic acid (H2C2O4) solution. Set up ring stand with an iron ring and wire gauze. Then set the Erlenmeyer flask on top of the wire gauze and, add a