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To run the synthesis of calcium oxalate via the precipitate from solution containing calcium ion and oxalate ion.2. To do a thermo gravimetric analysis on calcium oxalate.3. Understand and practice the method of homogeneous precipitation

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Introduction

FACULTY OF SCIENCE ANG ENGINEERING CHEMISTRY LABORATORY UESC 1122 Experiment 23 Synthesis and thermal analysis of the group 2(IIA) metal oxalate hydrates DATE : 10 NOV 2005 Objective : 1. To run the synthesis of calcium oxalate via the precipitate from solution containing calcium ion and oxalate ion. 2. To do a thermo gravimetric analysis on calcium oxalate. 3. Understand and practice the method of homogeneous precipitation through this experiment. Introduction Thermo gravimetric analysis (TGA) is one of the common analytical thermal analysis techniques that widely use to determine the thermal profile and stability of compound. This is rather important in the industry. When the thermal profile of certain substance was know, it can be produce in large quantity by an accurate reaction with the lowest cost. With the TGA techniques, a sample of material is being heated, while the sample mass is recorded as a function of temperature. By doing so, the composition of the material is analyzed, both qualitatively (which components are present in the material) and qualitatively (how much of these components is present). In this experiment, synthesis and thermo gravimetric analysis of calcium oxalate has been carried out. Synthesis of calcium oxalate was done by the reaction between calcium ions and oxalate ion: Ca2+(aq) ...read more.

Middle

Molecular weight of CaC2O4 .H2O= [40.0780+(2x12.0107)+(4x15.9994)+ (2x1.0079)+15.9994 ] = 146.1123 The mass of CaC2O4 .H2O produced = 2.5278 x 10-4 x 146.1123 = 0.03693g. The actual mass of CaC2O4 .H2O produce in this experiment cannot be calculated because the mass of the filter paper was not measured at the beginning, therefore the mass of filter paper cannot be subtracted from the total weigh of product and filter paper. It is recommended that each time running the experiment which involve the filtration, the mass of filter paper need to be measured. Discussion : 1.Generally, the reaction between the calcium carbonate and hydrochloric acid will produce the calcium chloride, water, and the carbon dioxide. CaCO3 + HCl CaCl2+ H2O + CO2 When calcium carbonate dissolved in acid, it gave up the Ca2+ ion into the solution which reacted with oxalate ions to form calcium oxalate in this experiment. 2. Methyl red (2-(4-Dimethylaminophenylazo) benzoic acid) is in form of dark red crystalline powder. It is stable compound and incompatible with strong oxidizing agents, thus it has been widely use as indicator in many types of titration. Methyl red has a transition range from pH 4.4 to pH 6.2. In more acidic condition it shows red colour, while in less acidic condition it will change colour to yellow. ...read more.

Conclusion

That is, use more reactant when perform this experiment, since the amount of reactant used is much, the weigh lost of yield product due to the error is negligible compare to total amount of the product, then the yield percentage can be calculate accurately. Besides that, a centrifuges can be used to helps to minimized the lost of calcium oxalates when collecting the precipitate. Conclusion: The theoretical mass of calcium oxalate should be produce in this experiment is 0.03693g and the yield percentage of product cannot be calculate since the weigh of product cannot be found. The very little of calcium carbonate used in this experiment makes the results be expected highly inaccurate. The calcium oxalate produce in this experiment is calcium oxalate monohydrate. Generally heating the solution below 70 oC will give the dehydrated salt while heating above 70 oC will give monohydrate salt. Reference: 1. Seamus P.J.Higson, Analytical Chemistry, 2003, 1st edition, New York: Oxford University Press, page 89-102. 2. David Harvey, Modern Analytical Chemistry, 2000, 1st edition, Singapore: Mc GrawHill International, page 255-262. 3. F.Albert Cotton, Geoffrey Wilkinson, Paul L.Gaus, Basic Inorganic Chemistry, 1995, 3rd edition, New York: John Wiley and Sons, Inc, page 307-315. 4. Thermogravimetry. Retrieved 14 November 2005, from WordReference.com English Dictionary web site: http://www.wordreference.com/definition/thermogravimetry 5. The Physical Chemistry behind the Periodic Table, from bbc.Co. Reproduction, 2005 web site: http://www.bbc.co.uk/dna/h2g2/A1013239 ...read more.

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