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Risk Assessment
Risk Assessment
1. Ensure that you are confident and safe in using a separating funnel for i) separation of mixtures and
ii) shaking reaction mixtures and realising any resultant pressure
2. Pour about 6.5 cm^3 of 2-methylpropan-2-ol into a 10 cm^3 measuring cylinder. 2-methylpropan-
2-ol is hazardous if inhaled so work in a fume hood.
3. Measure the mass of the measuring cylinder and contents.
4. Pour the 2-methylpropan-2-ol into a 250 cm^3 conical flask.
5. Measure the mass of the empty measuring cylinder and use this to record the exact mass of 2-
methylpropan-2-ol you have put in the separating funnel.
6. Using a 50cm3 measuring cylinder, measure about 20 cm^3 of concentrated hydrochloric acid.
Concentrated hydrochloric acid causes burns and his vapour irritates the lungs so use gloves and
work in a fume hood.
7. Over a period of about 2 minutes, add the concentrated hydrochloric acid GRADUALLY to the 2-
methylpropan-2-ol in the conical flask. The reaction is exothermic so be aware of pour it gradually.
8. Place a mineral wood plug into the neck of the conical flask and gently swirl the mixture every few
minutes.
Part 2: Separation
1. Using a funnel, pour the reaction mixture into a separating funnel. ENSURE THE TAP IS CLOSED SO
AS NOT TO SPILL THE CONTENT.
2. Allow the separating funnel to stand until the two layers have separed.
3. Open the tap and run the lower aqueous layer into a clean 100 cm^3 conical flask
4. Slowly add 10 cm^3 of 5% sodium hydrogencarbonate solution to the organic layer in the
separating funnel.
5. Put the stopper in the funnel and shake the contents gently. Carefully release the pressure build up
in the separating funnel.
6. Shake the contents more vigorously and again release the pressure. MAKE SURE THE FUNNEL IS
CLOSED.
7. Allow the two layers to separete, then remove the stopper and run off the lower aqueous layer as
in step 2 of part 2.
8. Repeat steps 3-7 until no more gas is given off.
9. Add 10 cm^3 of distilled water to the separating funnel and shake again.
10. Allow the layers to separete and then run off the lower aqueous layer – you can discard this layer.
11. Allow the organic layer to run into a clean 100 cm^3 conical flask. This liquid contains the product
of the reaction.
12. Anhydrous sodium sulfate acts as a drying agent to remove any traces of water. Add small
quantities (½ spatula measures at the time) to the organic liquid. Swirl between each addition to
the flask until the liquid is completely clear and the soduim sulfate no longer forms clumps.
Part 3: Distillation