CHM3301

NAME: NUR SYAHIRA MOHD YUSOF MATRIX NUM: 158144 PARTNERS NAME: NUR SHAFIKA RAHIM MATRIX NUM: 157537 EXP NUM: 5 TITLE: Complex Compound (The preparation and analysis of potassium trioxaluminate) DATE: 17.10.2011 DEMONSTRATERS NAME: NURUL ASIKIN HAJI MIJAN LAB: LECTURERS NAME: DR.TAN KAR BAN GROUP: 1

Experiment 5 Title: Complex compound of Aluminium (The preparation and analysis of potassium trisoxatoaluminate) Objectives: 1. To synthesis complex compounds of aluminium derived from sulfates and oxalates. 2. To determine the oxalate concentration and compare the reaction of aluminate complex with various reagents. Introduction. Aluminum is the third most abundant element after oxygen and silicon and also, the most abundant metal in the Earths crust. Aluminium presence in clays and alumino silicates mineral. Aluminum metal is too reactive chemically due to the bonding with oxygen to occur natively, it has a low density, insoluble in water, and its a very useful catalyst. Aluminium is commonly found combined with over 270 different mineral. The ore of aluminium is bauxite. Aluminium is called a complex compound because of a metal ion located at its centre together with additional molecules or ions nearby, which can be attached to other central ion by coordinate bond or also called as dative bonds. The atomic number of aluminium is 13 and the valence electron configuration of aluminium is nsnp in the p block. An aluminium have a remarkable low metal density and ability to resist corrosion, due to a thin layer of aluminium oxide that eventually formed when it is exposed to open air. The characteristic of the strongest aluminium alloys is the less corrosion resistant which is due to the galvanic reactions with alloyed copper .Due to the high melting point of the aluminum, which about 3600 F, enable the aluminum oxide to undergoes electrolysis. The refining of bauxite in the Bayers process of Karl

Bayer, will obtained white powdered aluminium oxide. The potassium trioxoaluminate contains aluminium in the complex compound form from the preparation of aluminium sulfate together with the mixture of sodium hydroxide and oxalic acid plus potassium oxalate. Aluminium is very useful in order to promote the blast power due to the reactive characteristic and also act as the catalyst and additive in chemical mixture.

Procedure: About 7 g of the hexadecahydrat (aluminium sulfate) were dissolved in 70 ml of water.By stirring,about 2.5 g of sodium hydroxide solutes in 10ml of water were added.

Then,the fresh Aluminium Hydoxide precipitate were filtered and washed with water. Oxalic solution was then prepared by diluting 4g of dehydrates and 6g of Potassium Oxalate in 70ml of water.The solution was then heated together with the filtered Aluminium Hydroxide until the volume reached 2/3 of the initial volume (more concentrated)

The undissolved Aluminium Hydoxide were then filtered.The filtrated were then cooled in the ice bath to allow crystallization.

As the crystal formed, it was then filtered and dried.

For analysis Determination of Oxalate.

2 g of the sample complex were dissolved in 100ml of 1M sulphuric acid. Then the solution was heated to 80 c.

Then the Oxalate was then titrated with 0.02M potassium permanganate solution,KmNo4 which has been standardized against 0.05M NaCO4 solution. The procedures were repeated three times.

Then,the sample (the crystal) and the aluminium sulfate were put on a test with four different reagents.About 2 ml of 4M Sodium Hydroxide,Sodium Acetate solution,Sodium Carbonate solution,and Sodium Orthophosphate solution were placed in a test tube each.Then a pinch of the salts were tested by dropping it to the each solution.The observation were recorded.The procedure were repeated with aluminium sulfate.

Result. 1) Mass of aluminium sulfate = 7.020 g 2) Mass of oxalic acid 3) Mass of oxalate = 4.012 g = 6.043 g

4) Mass of potassium trioxaluminate = 0.313 g Test Tube Result. Test with Aluminium Sulfate Reagent 4M Sodium Hydroxide Observation White cloudy color Have precipitate Sodium Acetate Clear solution obtained Sodium Carbonate Buble gas formed White cloudy color Have precipitate Sodium Potassium

Orthophosphate Permanganate White cloudy color Have precipitate No reaction occurs

Test with Potassium Trioxaluminate Reagent 4M Sodium Hydroxide Observation White cloudy color Have precipitate Sodium Acetate Sodium Sodium Potassium

Carbonate Buble gas Clear solution formed obtained White cloudy color Have precipitate

Orthophosphate Permanganate White cloudy color Have precipitate

Light pink color obtained

The titration table. First 24.30 ml 36.50 ml 12.20 ml Second 0.00 ml 12.10 ml 12.10 ml Third 13.10 ml 25.10 ml 12.00 ml 12.10 ml

Initial Reading Final reading Volume used Average

Average of volume used = (12.20 + 12.10 + 12.00)ml /3 = 12.10 ml

Calculation. Al2(SO4)3 + 6 NaOH 2 Al(OH)3 + 3 Na2SO4 2 K3( Al(C2O4)3) + 6 H2O 2 Mn2+ + 10 CO2 + 8 H2O

2 Al(OH)3 + 3 K2C2O4 + 3 H2C2O4 16 H+ + 2 MnO4 - + 5 C2O4 2-

Aluminium sulfate Mass= 7.020 g Mr = 666.42 g/mol

Mole = mass/Mr = 7.020 g / 666.42 gmol = 0.0105 mol ( A ) Ratio = 1:1:1 (from the equation)

Moles of Al(OH)3 = 2 A = 2 (0.0105 mol) = 0.021 mol Mole ratio of Al(OH)3 = K2 [ A/ (C2O4 )] .3 H2O With ratio of 1 : 1 Mol of 2 A = Metal complex Mass of Potassium Trioxalumintae = 2 (A) x Mr (theoretically) Mass of Potassium Trioxaluminate = 0.021 mol x 666.42 g/mol = 13.99 g ~ 14.00 g Percentage yield of Potassium Trioxaluminate = (experimental mass / theoretical mass) x 100 Mass of potassium trioxalate (exp) = 0.313 g % yield = (0.313 g/ 14.00 g) x 100 = 2.235 % g. Discussion. The proposed of this experiment is to synthesis the complex compound of aluminium derived from sulfates and oxalates and to determined the oxalate concentration. Few techniques were done to conduct this experiment such as, filtration and heating. Since aluminium occurs as aluminosilicates minerals and bauxite in natures, the electrolysis after dissolving the molten crylite can formed the aluminium metal. In the experiment conducted, the 70 ml of the aluminium sulfate have been dissolved with the sodium hydroxide, potassium oxalate and the oxalate acid. Then the solution were been stirred and heated, during the heating, the solution were ensured not to be boiled vigorously and heated not more than 80 c, the reason to do so is to ensure the ion complex in the solution does not

hydrolyze and decompose, the solution is needed to be boiled till up to 2 per 3 from the initial volumes of the solution left or less, to be accurate the solution need to be more concentrated. This is to ensure the preferred complex ion to exist more than the impurities and others ions, so when it is been cooled enough completely in the ice bath, more crystal can be formed. During the cooling,(crystallization) the longer the cooling process, more crystal will be formed. During the filtration, its advisable not to wash the precipitate with distilled water, since the ion is too small and easily washed out from the filter. The product yielded was then left to dry in oven and weighed. The product were used to determine the oxalate by titration and their reaction towards four of given reagents, the 4M sodium hydroxide, sodium acetate, sodium carbonate solution, sodium orthophosphate solution and potassium permanganate. The weight of the product yielded is 0.313g.The product yielded is low compared to others due to the errors done during the heating, the solution were heated more than 80c which allows the preferable ion decompose and were not concentrated enough to encourage the ion complex to undergoes crystallization during the cooling. The solution was too diluted. From the test tube test with the five given reaction,the first experiment,conducted by using aluminium sulfate powder.The crystal were sprinkle in the test tubes containing the reagents and the changes is observe,the reaction of the aluminium sulfate with the 4M Sodium Hydroxide,give a white cloudy color with a precipitation solution,a clear solution is observed when the crystal is sprinkled into the Sodium Acetate solution,the crystal dissolved in the solution,then,when the crystal sprinkled into the Sodium Carbonate,bubble gas formed and a whitish cloudy color and precipitate solution was observed after that,the crystal also give whitish cloudy color and precipitation solution when reacted with Sodium Orthophosphate,and when reacted with the Potassium Permanganate,there is no reaction occurs since there is no change.

Then,the product yielded,was tested,(Potassium Trisoxaluminate),using the same reagent and been compared,the observation made was likely the same with the test using Aluminium Sulfate except the Potassium Permanganate.it give a pinkish color when the product were sprinkled into the solution.The rest is the same,as the product give a whitish cloudy colour to the solution and precipitate when sprinkled into the 4M Sodium Hydroxide and to the Sodium Orthophosphate solution,while buble gas and white cloudy color and precipitate in the reaction with Sodium Carbonate.There is a clear solution formed when reacted with the Sodium Acetate. Precaution. 1) Do not boil the solution vigorously and ensure the temperature does not exceed 80 c in order to prevent the complex ion to decompose. 2) Place two filter paper on the Buchner Funnel to reduce the risk of the complex ion to filtered through the funnel (the ion is small) 3) Do not wash the precipitate with distilled water,to reduce more ion to hydrolyze and soluble. 4) Ensure the solution not to diluted,heat the solution to concentrated level to increase ion formation 5) Cool the solution in cold iced water to increase the crystallization,the longer the cooling,more crystal will formed Conclusion. 1) The Potassium Trioxaluminate yielded is 0.313 g 2) The percentage of product yielded is 2.235% 3) The percentage error is 1.1%

Refrences 1) Inorganic chemistry, Shriver & Atkins, fifth edition, 2010, 2) http://www.chemguide.co.uk/inorganic/complexions/whatis.html 3) www.ums.edu.my/sst/kimia/inorganik2.doc