EXPERIMENT II. [Cu{(H 2 N) 2 CS} 3 ] + (aq)

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1 EXPERIMENT II STABILIZATION OF RARE OXIDATION STATE-TRIS(THIOUREA) COPPER(I) SULFATE When an element can exist in more than one oxidation state in aqueous solution, each oxidation state will have different thermodynamic stability. In this experiment, two examples of the stabilization of an unusual oxidation state of copper will be studied. The stability of Cu I, which is generally less stable in comparison to Cu II in aqueous solution, will be achieved by complex formation using thiourea ligand that can function both as -bond donor and π-bond acceptor. It is to form stable complexes due to the neutrality principal. Thiourea can coordinate to the metal via the sulphur atom. Experiment 2-1: 16 Cu 2+ (aq) + 8 (H 2 N) 2 CS (aq) + 16 H 2 O (l) 16Cu + (aq) + S 8(s) + 16 NH 4 +(aq) + 8 CO 2(g) Cu + (aq) + 3(H 2 N) 2 CS (aq) [Cu{(H 2 N) 2 CS} 3 ] + (aq) Preparation of Tris(thiourea) Copper (I) Sulphate Prepare a solution of thiourea I (2.5 g in 15 ml of water) and a solution of copper (II) sulphate pentahydrate II (2.5 g in 15 ml of water) at room temperature. Cool the solution II in an ice-bath. Gradually and slowly add the solution II to solution I while stirring continuously. Allow the mixture to stand in the ice bath until white crystals or oily drops can be observed. Prepare another solution of thiourea (1 g in 10 ml of water), and add this solution to the cool reaction mixture while stirring vigorously. Allow the final mixture to stand for a while before filter the white crystals using a Hirsch funnel. Recrystallization Prepare a solution of thiourea (0.15 g in 30 ml water) containing a few drops of 1M sulphuric acid, and use this solution to dissolve the crude product while heating. During the recrystallization the temperature should not exceed 80 0 C (maximum of 75 o C to dissolve the product). The obtained solution is then filtered through a pleated filter. The filtrate may also be heated until any precipitated crystals have dissolved (a little colloidal sulfur passes the filter, so the solution will not become completely clear). The solution is cooled down afterward to room temperature by standing for 2-3 h. The crystals are collected by

2 filtration with suction, washed with 5 ml portion of cold water, followed by 5 ml portion of alcohol and dried in air overnight. Record the yield of the title compound in gram. Calculate the theoretical yield in gram and the actual yield in percent. Note that this is one of the general methods of preparing compounds containing a metal in a low oxidation state. The ligand in this case thiourea also functions as reducing agent, and the product in this case is obtained as the dehydrate. Complementary Work and Questions: 1. Prepare a solution of thiourea (1 g in 1M HCl 10 ml). Add a little copper powder and warm gently. Repeat the experiment without thiourea. Comment. 2. What is the reducing agent in the above preparation? Experiment 2-2: Determine the percentage of sulfate in the product from Experiment 2-1 Ba 2+ + SO 4 2- BaSO 4 NH 2 CSNH 2 + H 2 O 2NH 3 + H 2 S + CO 2 Note that the complex must be decomposed before determining the sulfate content, otherwise on the addition of barium chloride a thiourea compound is also precipitated. The complex is readily destroyed by making use of its sensitivity to hydroxyl ion attack. The product was recrystallized from acidified solution. Thiourea is also hydrolyzed by alkali. Weigh out accurately about 1.00 g of the solid complex into a 250 ml beaker, provided with a stirring rod and clock-glass cover. 50 ml of 2M NaOH are added, and the mixture is heated until the evolution of ammonia has ceased (~30 mins). The copper precipitates as the sulfide. Filter and wash with cold water. Acidify the combined filtrate and washings with 2M HCl. Heat the solution to boiling. Add warm 5% barium chloride solution (5 g BaCl 2.H 2 O in 100 ml of water ca. 0.2M) drop wise using an eyedropper ml. Stir the solution constantly during the addition. Allow the precipitate to settle for a

3 minute or two, before test the supernatant liquid for complete precipitation by adding a few drops of barium chloride solution. If a precipitate is formed, add slowly a further 3 ml of the reagent. Allow the precipitate to settle as before and test again. Repeat the operation until an excess of barium chloride is present. When an excess of the precipitating agent has been added, keep the covered solution hot, but not boiling for an hour (steam bath, low temperature hot plate) in order to allow complete precipitation. The precipitate should settle readily, and a clear supernatant liquid should be obtained. Test the latter with a few drops of barium chloride solution for complete precipitation. If no precipitate is obtained the barium sulfate is ready for filtration using sinter glass (no. 4). Dry the precipitate in the oven at C. Calculate the percentage of SO 4 in the sample. Determination of copper in the product from Experiment 2-1 Prepare standard 0.01M Na 2 H 2 (EDTA) solution Dry approximately 4.0 g of Na 2 H 2 (EDTA).2H 2 O [M= gmol -1, H 4 (EDTA) = (HOOC) 2 CH 2 CH 2 (COOH) 2 ] for 2 h at 80 0 C and cool in a desiccator. Accurately weigh and dissolve in deionized water using 1000 ml volumetric flask. Prepare Buffer solution Dissolve 17.5 g NH 4 Cl in 142 ml conc. NH 4 OH and dilute to 250 ml with distilled water. Standardization of the EDTA solution with 0.01 M CaCO 3 Pipette 25.0 ml of 0.01M CaCO 3 into 250 ml Erlenmeyer flask. Add approximately 25 ml of deionized water followed by 2.0 ml of ph 10 buffer solution and a small quantity of Erichrome Black T indicator powder, swirl the solution to dissolve the powder (1 g Erichrome Black T in 100 g NaCl). The solution should appear wine red. Titrate the solution with the 0.01M Na 2 H 2 (EDTA) solution until the color changes from red to a pale blue (end point). Repeat this procedure at least twice. Calculate the concentration of the Na 2 H 2 (EDTA) solution.

4 Analysis of the complex for copper Cu 2+ (aq) + H 2 (EDTA) 2- (aq) Cu(EDTA) 2- (aq) + 2 H + (aq) Weight approximately 0.10 g of the complex into a 250 ml beaker with as little water as possible. Slowly add 5 ml of conc. HNO 3 to the powder and 20 ml of DI water. The mixture is heated until the evolution of nitrogen oxides has ceased. Allow the beaker and its contents to cool to room temperature. The sample solution is transferred to 250 ml Erlenmeyer flask, wash the sides of the flask with small amount of water and adjust the volume to approx. 50 ml with water. Add conc. ammonia solution dropwise to the solution, until the solution has turned blue color. Add a little murexide indicator ( g) and titrate the solution with the 0.01M Na 2 H 2 (EDTA) solution until the indicator changes from green to violet. What mass of the compound contains one mole of copper? Complementary Work and Questions: 1. From the available infrared spectrum of the product, identify as many group frequencies as you can. 2. Draw the structure of the product. References 1. G. Pass and H. Sutcliffe, Practical Inorganic Chemistry, Chapman and Hall, London, N.V. Sidgwick, The Chemical Elements and Their Compounds, Oxford University Press, Oxford, K. Swaminathen and H.M.N.H. Trving, Inorg Nucl. Chem., 1964, 26, J.V. Quagliano, et at., J. Amer. Chem. Soc., 1958, 80, A.J. Vogel, A text book of Quantitative Inorganic Analysis, 3 rd edition, Longmans, London, (or new editions). 6. B.A. El-Sayed and M.M. Sallam, Temperature and frequency dependent electrical transport in thiourea and tris(thiourea) coupper (I) sulphate, J. Mater. Sci.: Mater. Electron., 1999, 10,

5 Infrared Spectrum of Tris(thiourea) copper (I) sulphate

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