The butyl bromide water mixture is then cooled by running the tap water through external wall of

flask. Next, the distillation apparatus is assembled and set up by clamping the round-bottomed flask
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to a retort stand and the connecting joint of the condenser and its exiting adapter to another at a
lower height. A conical flask is placed below the exiting adapter to collect the distillate while the
electrothermal heater is placed below the round-bottomed flask containing the mixture. The
Preparation of n Butyl Bromide Download AI Quiz
thermometer together with its adapter is made sure that its bulb is placed right at the junction of the
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side-arm of the still distillation head. Water is run through the condenser from the pipe with the
inlet near the exiting adapter and the outlet near the side-arm of the still head. The mixture is
distilled out until no further oily drops appear in the condenser.

On the other hand, the separating funnel is suspended using a supporting ring clamped to a retort
stand. The distillate collected is placed into the separating funnel with the stopcock tap closed. The
funnel stopper is inserted into the mouth of the funnel, which is left for a few minutes for the
organic and aqueous layers to form. A conical flask is placed under the funnel. The stopcock tap is
then opened and the lower layer of crude butyl bromide is run off into the conical flask and the
upper aqueous layer is drained off into a different flask. After that, the crude bromide is returned to

the separating funnel. 15mL of concentrated HCl is measured and added into the funnel. The funnel
is closed with stopper, and left few minutes to form two layers. If some organic layer trapped above
the aqueous layer, the mixture is shaken gently with both hands, which is later inverted with finger
over stopper and the stopcock tap is opened to release the pressure inside the stopper, i.e. a hissing
sound of gas released is heard. The funnel is then put back into the ring and the lower layer is
drained off into the conical flask by opening the stopcock. The upper layer is then run off into
another flask. The washing step is then repeated by adding 25mL of water, 20mL of 10% sodium
carbonate solution and 25mL of water successively into the funnel. In all cases the bromide is the
heavier, lower layer.

Next, about three spatula of anhydrous calcium chloride is added into the flask to dry the product
for about 10 minutes, with occasional shaking. After that, , a filter paper is folded into fluted form
and inserted into a stemless glass funnel and the product is filtered via gravity filtration into an
empty, clean 50mL round bottomed flask. 2 to 3 boiling chips are added into the flask.

Next, the Liebig condenser, the exiting adapter and 50mL round bottomed flask are washed with
acetone. The distillation apparatus together with the round-bottomed flask is assembled again for a
second distillation. An empty glass vial together with is cap is weighed and its mass is recorded.
The contents of the beaker are heated and the temperature is observed. Any distillate produced
before 97°C is collected into an empty beaker. Distillate produced in the range of 97-103°C is
collected into the vial (an extra vial is prepared if the first vial is unable to collect the distillate
within the range). The vial is capped as soon as possible after the product is collected since the n-
butyl bromide is volatile. Any distillate produced after 103°C is collected in another beaker. The
vial is weighed to obtain the net mass of the distillate and labelled with details of the experimental
results.

SPACE FOR PROCEDURE DIAGRAM