MAJORCHEMLAB - Synthesis and Analysis of K3Fe(C2O4)33 H2O...

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Synthesis and Analysis of K 3 Fe(C 2 O 4 ) 3 •3 H 2 O Suman Mahmood November 24, 2015 Dr. Brack
Introduction: These series of experiments involved the synthesis of potassium ferric oxalate and the verification of the purity of the product we created. This experiment was split into three laboratory periods. During this experiment we determined the Percentage Oxalate Ion in the potassium Ferric Oxalate Trihydrate sample using titration. This will involve adding Potassium Permanganate solution, to a solution of the Oxalate until the reaction between these species is complete. By knowing the reaction stoichiometry, the volume Permanganate Ion solution required, and the concentration of the solution used, we can determine the amount of Oxalate Ion present in our sample. This will allow us to confirm the solid we have generated is the trioxalate of Iron. Procedure: Part 1: Synthesis of an Iron Compound 1. On an analytical balance, accurately measure 5 g of ferrous ammonium sulfate, Fe(NH 4 ) 2 (SO 4 ) 2 •6H 2 O. Record the exact mass in your notebook 2. Obtain 15 ml of deionized water in a clean squeeze bottle and transfer the deionized water to a clean 250-mL flask. 3. Add the 5 g of ferrous ammonium sulfate to the 150-ml beaker and stir to dissolve. 4. Add 5 drops of 3 M H 2 SO 4 to the solution of ferrous ammonium sulfate. Stir to mix. 5. Clamp the 250-ml flask to a ring stand and support the flask with an iron ring and wire gauze. Heat the mixture to boiling. Be sure to continuously stir the contents to prevent bumping. 6. Turn off the Bunsen burner. Carefully remove the 150-ml beaker using crucible tongs or the utility clamp.
7. Continue stirring the beaker contents as they cool to prevent “bumping.” 8. Obtain a beaker and decant the supernatant liquid in the 250-ml flask into the beaker. There should be a yellow solid remaining. 9. Return the flask to the ring stand and add approximately 20 ml of deionized water. Heat the solution but do not allow the solution to boil. 10. Let the solid settle as before and decant the liquid yet again into a beaker. 11. Add 10 of a saturated potassium oxalate solution to the yellow solid remaining 12. Obtain 20 m of 3% H 2 O 2 in a beaker and 8 ml of 1M H 2 C 2 O 4 in a graduated cylinder.

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