SKT EXP1 N 2.docx - TITLE Synthesis of oxalate Complexes of...

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TITLE : Synthesis of oxalate Complexes of Iron & Characterization of Oxalate Complex of Iron. OBJECTIVE EXPERIMENT1 1. To synthesis iron(II) oxalate, FeC 2 O 4. 2. To synthesis potassium trioxalatoferrate(III) trihydrate, K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O. EXPERIMENT 2 To learned how to analyse and determine of oxalate complex using: 1. Infrared spectroscopy. 2. Microelemental analysis.
METHOD: Part A Preparation of Iron (II) Oxalate, FeC 2 O 4 1. 1.0 ml 2M sulphuric acid was added into 50.0 ml warm water, followed by 15g ferrous ammonium sulphate. 2. 10% oxalic acid solution was prepared. Then, a solution of 10% oxalic acid (75.0 ml) was added slowly with rapid stirring. PRECAUTION This step must be conducted in fume hood. 3. The mixture was gently heated until boiling. 4. Turn off the heat and brought the mixture to room temperature and wait the yellow precipitate of ferrous oxalate to settle down. 5. The precipitate was removed by vacuum filtration. Washed it thoroughly with hot water (3x10.0ml) followed by acetone (3x10.0 ml). 6. The product was dried in a desiccator and weighed. This product will be used to synthesised potassium trioxalatoferrate(III) trihydrate. Part B Preparation of Potassium Trioxalatoferrate(III) Trihydrate, K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O 1. A potassium oxalate solution was prepared by add 2.306 g of potassium oxalate monohydrate in 10ml warm water. 2. Then, 1.125 g of iron(II) oxalate (product from Part A) was added into the potassium oxalate solution. 3. The solution was heated and maintained the temperature at 40°C. 8 ml of hydrogen peroxide was added dropwise (H 2 O 2 , 30% v/v) while the solution is stirred continuously. The solution should contain a precipitate of ferric hydroxide. PRECAUTION This step must be conducted in fume hood. 4. Then, the solution was heated until boiling. 5. 10% oxalic acid (5 ml) was drop wisely until the precipitate just dissolves. During the addition of oxalic acid, the solution’s temperature should be maintained near the boiling point. 6. The hot solution was filtered by vacuum filtration and add ethanol (8 ml) to the filtrate. If there are some crystals formed, re-dissolved those crystals by gentle heating and stir the solution by using the glass rod.
7. The solution was put in a dark cupboard to crystallize. PRECAUTION Product is photosensitive. 8. The solution was filtered by using a Buchner funnel and collect the crystals. Washed them with an equal volume mixture of ethanol and water. 9. Dried and weighed the product. 10. Kept the product in the dark environment. PRECAUTION Product is photosensitive. Part C Analysis of Oxalate Complex by Infrared Spectroscopy and Microelemental Analysis 1. Used FT-IR spectrometer to get the IR spectrums for iron(II) oxalate, potassium trioxalatoferrate(III) trihydrate and oxalate acid (ligand). 2. Used elemental analyser CHNS-O to get microelemental data for iron(II) oxalate, potassium trioxalatoferrate(III) trihydrate and oxalate acid (ligand).

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