Chem 121L: The Synthesis of Ferric Oxalate Trihydrate and the Determination of Composite Oxalate Ion

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CHEM 121L Section 7 October 5, 2017 The Synthesis of Ferric Oxalate Trihydrate and the Determination of Composite Oxalate Ion This procedure’s main purpose was to synthesize Ferric Oxalate Trihydrate through a process of various oxidations and reductions achieved through mixing and heating. First produced was a sample of Ferric Oxalate Trihydrate, then its purity was tested through titration. Introduction In chemistry, it is very important to track the conversion of reagents to their relative products through stoichiometry in chemical reactions. Through doing this, charges of products and reagents can be known and therefore the dynamics of the reaction can be studied. In this lab, the various chemical and physical properties of multiple substances are used to combine and separate them, to ultimately synthesize a desired product, in this case Ferric Oxalate Trihydrate. It was then tested for accuracy through titration using a Permanganate solution. Procedure For the Synthesis of Potassium Ferric Oxalate Trihydrate First, Ferrous Oxalate Dihydrate was produced 5g of ferrous ammonium sulfate hexahydrate was added to 15mL H 2 O and 3M H 2 SO 4 . The solution was then added to 25mL of H 2 C 2 SO 4 . The solution was then heated until boiling, stirred, and allowed to settle. Then the solution was turned into Potassium Ferric Oxalate Trihydrate After decanting the substance again with 25mL H 2 O, 10mL K 2 C 2 O 4 was added. The solution was heated to 40oC, and 20mL 3% was added slowly. This was then filtered and allowed to cool, with 10mL ethyl alcohol added. The precipitate was then allowed to sit for a week, when removed it was filtered again, the remaining precipitate being the Ferric Oxalate Trihydrate. For the Standardization of the Permanganate Solution: The buret was prepared and filled with KMnO4 solution.
Approximately 0.11g Na 2 C 2 O 4 was weighed on glazed weighing paper using an Analytical Balance The Sodium Oxalate was transferred to a 125 mL Erlenmeyer flask and 30 mL of deionized Water and 5 mL of 6M H2SO4 were added. The sample was heated to about 60 O C over a direct flame While still warm, the sample was titrated with the Permanganate solution until a pink color persisted for about 30 seconds For the Titration of Potassium Ferric Oxalate Trihydrate 3 samples of 0.1g Potassium Ferric Oxalate Trihydrate 0.1g were prepared. Each sample was added to a 125 mL Erlenmeyer flask with 30 mL deionized Water and 5 mL 6M H2SO4 The solutions were then heated to about 60 O C. The samples were then titrated in the same way as the Sodium Oxalate. Data For the Synthesis of Potassium Ferric Oxalate Trihydrate Weight of Ferrous Ammonium Sulfate Hexahydrate used to create Ferric Oxalate Trihydrate: 4.9998g For the Determination of Oxalate Ion in Ferric Oxalate Trihydrate The below tables record the weights, start points and endpoints of the titrations performed Sodium Oxalate Titration Weight Start Point End Point Sample 1 0.1114g 0.50mL 30.90mL Sample 2 0.1113g 1.25mL 34.18mL Sample 3 0.1146g 3.66mL 38.74mL
Ferric Oxalate

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