Synthesis and Characterization of an Oxalate Compound.docx

Synthesis and Characterization of an Oxalate Compound.docx...

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Synthesis of an Oxalate Compound Introduction: In this particular activity, you will be making an oxalate compound to analyze in a later lab exercise. It is necessary to make this compound ahead of time such that compound is allowed to dry before analysis. Background: The compound that you will be making will have the general formula of: M x (C 2 O 4 ) y zH 2 O. The value of M will be one of the three metals – iron (Fe), cobalt (Co), or manganese (Mn). The variables of x, y, and z will be determined in a subsequent lab activity. It should be mentioned that this compound is an example of a hydrate, where the water molecule(s) occupy spaces within the crystal lattice. Thus, the ratio of water molecules is fixed and this water content can often be determined by heating the hydrate. However, in this case the compound also undergoes pyrolysis, which converts the hydrate to an oxide. The reaction will use one of two possible metal ions as a chloride salt and then mixed with a solution of oxalic acid (1) or (2). Both products will be distinctly different in their appearances due to the metal. (1) x CoCl 2 6H 2 O + y H 2 C 2 O 4 + z H 2 O Co x (C 2 O 4 ) y zH 2 O (2) x MnCl 2 4H 2 O + y H 2 C 2 O 4 + z H 2 O Mn x (C 2 O 4 ) y zH 2 O The compound that forms is insoluble in water, which will allow you to collect it by filtration. Procedure: 1. Your instructor will assign each group the metal salt they will be using for this experiment. Make sure to record its formula and determine its molar mass (including the water molecules!) accurately to two decimal places. 2. On a weighing boat, measure out about ______ g* of your salt and record the actual mass to 0.001g. *For the Mn salts, use about 3.3g; for the Co salt, use about 4.0g. 3. Add your solid salt to about 20 – 25mL of distilled water in a 50-mL beaker and stir with a stir rod until dissolved. While you are waiting, calculate and record the moles of your salt to the correct number of significant digits. 4. In a 50-mL graduated cylinder, measure out between 48 – 50 mL of 0.750M H 2 C 2 O 4 (oxalic acid) and record the actual amount to the nearest 0.1 mL. Transfer the solution to a 250-mL beaker. 5. Slowly add the metal salt solution in the 50-mL beaker to the oxalic solution in the 250-mL beaker with constant stirring. This step should take from three to five minutes to complete. 6. Place your beaker along with a second one containing approximately 20 mL of distilled water for ten minutes in the community ice bath to cool. If there are many groups, then you may want to label your beaker. While you are waiting, calculate and record the moles of oxalic acid that you used. 7. Collect the product via suction filtration on a piece of filter paper. Add the liquid and solid slowly to the suction filter. Use your additional beaker of cold water to rinse any remaining solids from the first beaker. Suction for five minutes after adding all of the liquid.
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  • Fall '09

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