Chem Labb.docx - Synthesis and Analysis of K3Fe(C2O4)3 3H2O...

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Synthesis and Analysis of K3Fe(C2O4)33H2OKristian GauvinNovember 19, 2018Chem 3B
Introduction:Purpose:The purpose of this experiment was to verify the purity of the potassium ferric oxalate compoundby first synthesizing the ferric oxalate and then analyzing the oxalate and iron percentages in thecompound.Chemistry:In the first part of this three-process experiment, the synthesis of potassium ferric oxalate-whichwill be broken down into two steps- was needed. To achieve this product, the synthesis ofanother compound called ferrous oxalate will be required. The synthesis of this compound is asfollowed:Fe(NH4)2SO4∙6H2O(aq)+ H2C2O4(aq)→FeC2O4∙2H2O(s) + 2(NH4)HSO4(aq)∙4H2O(s)This product is an insoluble opaque yellow solid solution, which is counter intuitive because thereactants of this solution are all soluble. In the next step, the ferric oxalate will be created by theoxidation of ferrous oxalate by the hydrogen peroxide. This reaction is shown here:2FeC2O4∙2H2O(s) + H2O2(aq) +H2C2O4(aq) + 3K2C2O4(aq) →2K3Fe(C2O4)33H2O(s)This reaction resulted in the production of a green crystal like solid, but due to its sensitivenature it was kept in a dark space.After this step, the amount of oxalate ion in the product wasdetermined by not only the reaction of the oxalate ion with potassium permanganate but also bythe titration of the solution. This reaction is as followed:5C2O4-2+ 2MnO4-+ 16H+ → 10CO2+ 2Mn+2+ 8H2O
Next, the concentration of the iron in the sample needed to be analyzed. To be able to determinethis, the iron in the product must be made into a new complex using the phenanthrolinemolecule. After doing so, the iron will then be reduced by hydroxylamine hydrochloride fromFe(III) to Fe(II). The reduction of Fe(III) and formation of Fe(II) by this compound, respectively,is shown:4Fe+3+ 2H2NOH → 4Fe+2+ N2O + 4H++H2OFe+2+ 3C12H8N2→ Fe(C12H8N2)3+2Then, the amount of light that is absorbed by this complex, by lining up to the standards ofBeer’s Law, will be used to show the amount of iron in the sample produced.Experiment: ProcedureThis three-week experiment was broken up into three separate experiments. For the first week, aring stand was set up and a Bunsen burner was added under it. Exactly 15 mL of deionized waterwas added to an empty 100 mL graduated cylinder. Using the scale, 5.2 grams of Fe(NH4)3wasweighed out and placed in a 150 mL beaker. Then, the deionized water was added with the 5.2grams, combined with 5 drops of 1.5M H2SO4. After these were added, it was swirled with astirring rod. The the resultant was poured into an Erlenmeyer flask. Clamped the flask at an angleover the unlit Bunsen burner. After cleaning the 100ml graduated cylinder, 25 mL of oxalic acidwas added to the cylinder and poured in the Erlenmeyer flask with the resultant. The solutionimmediately turned an opaque yellow. After mixing, the Bunsen burner was ignited, and theliquid was heated enough but not to a boil. The Bunsen burner was turned off and waited for the

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Term
Fall
Professor
DR.BINDRA
Tags
Laboratory glassware, Erlenmeyer flask, oxalic acid, oxalate

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