Experiment 17 Topic : Technique - synthesis.

Purpose : To determine the percentage of aluminium in a sample Xby means of the preparation of a complex compound of aluminium with 8 hydroxyquinoline. Materials : KA 1 is a solution of 8 hydroxyquinoline in ethanoic acid. KA 2 is 2.0 mol dmaqueous ammonium ethanoate. KA 3 is sample X. KA 4 is 2.0 mol dmhydrochloric acid. Apparatus : Electric balance 0.01g (common use). Oven (common use). Magnetic stirrer. One 250cm beaker. One 50cm measuring cylinder. One Bunsen burner. One tripod stands and wire gauze. One retort stand and clamp. One thermometer 0 C to 100 C. One crucible and lid. One filter tuner and filter paper. One wash bottle filled with distilled water. Introduction : Aluminium in a certain sample can be determined quantitatively by means of the process of formation of complex compounds, for example, an alum complex is produced by the reaction of an alum with 8 hydroxyquinoline. Procedure : (a) Weight out accurately between 0.25g and 0.30g of KA 3 . The readings are recorded in the table below. Mass of container + KA 3 / g Mass of empty container / g Mass of KA 3 / g 104.69 104.43 0.26

All of the KA 3 are placed into a 250cm beaker, and 150cm of distilled water are added followed by one drop of KA 4 . The mixture is warmed to a temperature between 60 C and 70 C. Then 25cm of solution KA 1 are added, slowly followed by 50cm of solution KA 2 . A precipitate will be formed. The beaker is removed. This solution is stirred for half an hour by using a magnetic stirrer. An empty crucible is weighed and the readings are recorded in the table below. The solution above is filtered and the precipitate is

washed with cold distilled water. The precipitate is transferred into an empty crucible and the precipitate is dried in the oven at about 120 C. The crucible is cooled and weighed together with its contents. Mass of crucible + precipitate / g Mass of empty crucible / g Mass of precipitate / g Question : (c) Explain. (i) Why the mixture of solutions KA 1 and KA 2 needs to be stirred for half an hour using the magnetic stirrer? To make the solution KA 1 and KA 2 to be uniform to get better reaction and transmit heat uniformly. (ii) Why the complex precipitate is washed with cold water? To separate out the fluorine particle with the pure precipitate. (d) How would you ensure whether the complex precipitate obtained is completely dried? First, randomly take the mass of precipitate in different time after 1 hour and then until get the constant mass to ensure the complex precipitate obtained is completely dried. (e) Calculate the mass of 1 mole of complex compound with the formula Al(C9H6NO)3. Mass = 27 + 3[9(12) + 6(1) + 14 + 16] = 27 + 432 = 459 g (f) Calculate the percentage of aluminium in the complex compound. 27_ Percentage of aliminium = 459 x 100 % = 5.882 % 30.43 30.28 0.15

(g) Calculate the percentage of aluminium in sample X. 459 g of Al(C9H6NO)3 contains 27 g of Al. 0.15 g of sample X contains Y g of Al.

27 x 0.15 Y= 459

Y = 0.00882 g

0.00882 Percentage of aluminium in sample X = 0.26 x 100 %

= 3.392 %

Conclusion : The percentage of aluminium in sample X is 3.392 %.

Comment :

(i) Temperature must be constant between 60 C and 70 C when continue the reaction to prevent error occurred. (ii) We should carry out technique synthesis in right way, do not need do not put too many salts into the distilled water.