TASK 1 (P7) OXIDISING ETHANOL TO ETHANAL Objective: To be able to control oxidisation by addition and distillation.

n. And also to be able to calculate the yield. SAFETY Wear eye goggles and gloves Ethanol and ethanal are flammable. Concentrated sulphuric acid is corrosive. Sodium dichromate (VI) is a class 2 carcinogen and ethanal is class 3- wear gloves. PROCEDURE 1. Slowly add 1.7cm3 of concentrated sulphuric acid to 5cm3 of deionised water in the boiling flask. It may be necessary to cool the flask down. 2. Set up the apparatus for preparation by distilling as shown in the diagram. 3. Prepare a solution of 5g of sodium dichromate in a mixture of 5cm3 of deionised water and 4.0cm3 of ethanol. Once all of the sodium dichromate has dissolved, pour the mixture into the separating funnel, making sure the tap is closed. 4. Connect the apparatus and start the water condenser. Heat the flask with a small flame and add the liquid from the separating funnel at the same rate as the liquids distils over and is collected. The collection vessel should be immersed in ice as ethanal is a volatile compound. 5. Measure and record the volume of the ethanal collected. Now carry out the chemical tests as described in steps 6 and 7. 6. To a portion of the distillate, add some of the universal indicator.

EQUIPMENT/MATERIAL Ethanol Concentrated sulphuric acid, H2SO4. Sodium dichromate (VI), Na2Cr2O7. Conical flask, beaker, spatula. Crushed ice, deionised/distilled water. 2 x 10cm3 measuring cylinder, spatula. Small Bunsen burner. Mass balance and weighing bottle. 50 cm3 quick fit round-bottomed flask, still head, dropping funnel, Liebig condenser, and delivery tube. Boiling tube and bung. Universal indicator and chart.

OXIDISING ETHANOL TO ETHANOIC ACID Objective: To be able to reflux. And also to be able to separate mixtures by distillation. SAFETY Wear eye goggles and gloves. Ethanol is flammable. Concentrated sulphuric acid is corrosive. Sodium dichromate (VI) is a class 2 carcinogen.

PROCEDURE 1. Slowly add 3cm3 of concentrated sulphuric acid to 5cm3 of deionised water in the boiling flask. It will be necessary to cool the flask with iced water as you add the sulphuric acid to the water. 2. Completely dissolved 5g of sodium dichromate in the mixture from step 1 and add a small amount of pumice. Do not proceed further until all of the sodium dichromate has dissolved. 3. Arrange the apparatus for reflux as shown in figure 1 and turn on the water for the condenser. 4. Make a mixture in a beaker of 1/2cm3 ethanol and 5cm3 of water and add this a little at a time through the condenser using iced water to cool the boiling flask as necessary. Note that this can be very violent and will need frequent cooling. 5. When all the ethanol solution has been added, heat the boiling flask on a water bath and reflux for 3o minutes 6. Allow the reaction mixture to cool. Now rearrange the apparatus for distillation as shown in figure 2. 7. Distil with a small flame and collect about 10cm3 of distillate. This should be aqueous ethanoic acid. EQUIPMENT/MATERIALS Ethanol Concentrated sulphuric acid, H2SO4. Sodium dichromate (VI), Na2Cr2O7. Conical flask, beaker. Crushed ice, deionised/distilled water. 2 x 10cm3 measuring cylinder, spatula. Small Bunsen burner. Mass balance. 100cm3 quick fit round-bottomed flask, still head, dropping funnel, Liebig condenser, and delivery tube. Boiling tube and bung. Pumice Gloves

). SYNTHESIS AND SEPARATION OF ASPIRIN PROCEDURE`0 1. Weigh out 3.0g of salicylic acid and place in a 250ml Erlenmeyer flask. 2. Measure out 6.0ml of acetic anhydride and add this to you flask. Be sure to do this in the hood and wear your goggles. Dont let the acetic anhydride contact your skin and dont get vapour in your eyes. 3. Carefully add 5 to 10 drops of 85% phorophoric acid, a catalyst, to the flask and swirl to mix everything thoroughly. 4. Still in the hood, heat the mixture for about 10 minutes in a beaker of warm water (70-800C). 5. After heating, cautiously add 20drops of distilled water 6. Next add 20ml of distilled water and cool in the ice bath. If crystals do not appears you can scratch the walls of the flask with a stirring rod to induce crystallization. 7. Then filter the solid aspirin through a piece of pre-weighed filter paper using a Buchner funnel and the aspirator. Wash the crystals with 2-3m of chilled water allow the air to be drawn through the solid and filter paper for 15 minutes. 8. Place the filter paper with the product in a watch glass and put it in the oven at 1000C for about 30mins till is dry. 9. Put the dry aspirin and filter paper into a pre-weighed plastic bag and weigh again 10. Measure the melting range with the Meltemp apparatus and compare to the value for pure aspirin of 138-1400C. 11. Calculate the weight of your product by subtracting the weight of the paper and bag form the total.

TASK 1 (P6)