Synthesis and Analysis of Potassium Ferric Oxalate Final Curse hero.docx

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Synthesis and Analysis of Potassium Ferric Oxalate Introduction: This lab experiment is a series of experiments that involve the synthesis of potassium ferric oxalate ( K 3 Fe(C 2 O 4 )3 3H 2 O ), from ammonium Iron Sulfate (Fe(NH 4 ) 2 (SO4) 2 *6H 2 O) and establishes the authentication of the composition and the pureness of the product that is created. The experiment covers three laboratory periods to prepare the compound. In the first laboratory period will prepare the compound, by the synthesis of an iron compound. The molecular equation for the synthesis of potassium ferric oxalate being Fe(NH) 2 (SO4) 2 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)+ 4H 2 O . Than it will sit and dry out for a week, creating crystals for week two. In week two laboratory period the product/ crystals will be filtered, dried, and weighed out. In the same period two solutions will be prepared for the
analysis of the composition of the product, and spectrophotometric analysis will be performed of the iron in the product. The product will be oxidized by hydrogen peroxide the molecular equation for the reaction is, 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). During week two the product is analyzed for iron (iii), through the reduction of iron by hydroxylamine, the reaction between the two is: 4Fe +3 + 2H 2 NOH-- 4Fe +2 +N 2 O+4H + +H 2 O. Also during the analysis of iron, the formation of iron (ii) is detected with phenanthroline, the reaction between the two being: Fe +2 +3C 12 H 8 N 2 Fe(C 12 H 8 N 2 ) 3 + . The final, third lab period is devoted to the analysis of the oxalate content of the product produced. The oxalate ion will produce a reaction with the permanganate ion in the reaction 5C 2 O 4 -2 +2MnO 4 - +16H + - 10CO 2 (g) +2Mn +2 +8H 2 O. Procedure #1: For the firsts week procedure of the lab 5.00 grams of ammonium sulfate, Fe(NH) 2 (SO4) 2 6H 2 O is added to 15.00 mL of deionized water in a 250 mL Erlenmeyer flask. After about five drops of three molar (3M) Sulfuric Acid (H 2 SO 4 ) is added. Than by swirling the flask everything in the solution will become dissolved. After the solid is dissolved add 25 mL of 1 molar (1M) oxalic acid (H 2 C 2 O 4 ). When adding the oxalic acid, the solution turns yellow. Then clamp the flask to a ring stand, and have the support of the flask with an iron ring. Underneath the flask have a wire gauze, and the set the Bunsen burner underneath. Start to heat the solution with the Bunsen burner until it starts to boil. Care is needed to ensure the solution does not boil over. The solution can be stirred with a glass rod while heating to help keep the solution from boiling over. Once the solution starts to boil, stop heating the solution, and let the solid set. After letting the solid set, take a pair of crucible tongs, or utility clamp to hold the flask and pour out the clear liquid into a beaker, leaving the yellow solid inside of the flask. The reaction to create
the yellow solid of Ferrous oxalate is Fe(NH) 2 (SO4) 2 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)+ 4H 2 O.

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