SUBLIMATION

Introduction

Some solids can easily change into vapours (volatilisation); these vapours (instead of
condensing into a liquid and the liquid freezing back to the solid) can sublime, that is,
the vapours form a solid without going through the liquid state. Even ice can be
volatilised and sublimed (needs to be at reduced pressure, 1/100th of the usual
atmospheric pressure). Volatilisation / sublimation is useful to purify some solids as
menthol, naphthalene, iodine, etc. Heat sensitive medicines and enzymes are dehydrated
by means of cooling them down until water freezes and ice formed can be sublimed.

Aims

To purify different substances by means of sublimation.

Apparatus

Tripod, wire gauze, Bunsen burner, beaker, watch glass, spatula, microscope, slides, and
coverlids, capillary tubes, thermometer, ice, water and samples.

Procedure

1- Put some iodine mixed with sand (sample 1) in a beaker and heat it
gently until violet vapours appear inside.

2- Stop heating and cover the beaker with a watch glass put some ice on the
watch glass to refrigerate and allow the vapours to deposit (sublime);
wait for some time and observe the crystals formed.

3- Gather them and keep them in a polythene bag. Observe them through a
microscope and draw what you see.

4- Do you think that iodine has been purified? How would you know?

5- Repeat all items from (1) to (3) using impure benzoic acid instead of iodine. Be
sure that the beaker is absolutely dry or humidity will condense on the watch glass
and the crystals will be spoiled.

6- Compare both the impure and the sublimed benzoic acid.

7- Now carry out a third sublimation but using your raw naphthalene sample from last
week’s experiment (Freezing and Melting).

8- After looking at the naphthalene crystals through the microscope, collect as much
sublimed naphthalene as you can in a clean watch glass.

9- Seal on end of a capillary tube but putting its tip on aflame. It gets red hot and after
some 3 – 4 seconds should be sealed. Show your teacher before you follow on.
10- Fill the capillary tube as described below

11- Pack the capillary tube by pressing the open end gently into a sample of the
compound to be analyzed. Crystals will stick in the open end of the tube.

12- The solid should fill the tube to a depth of 2-3 mm. Tap the bottom of the capillary
on a hard surface so that the crystals pack down into the bottom of the tube

13- Fix the capillary to a thermometer (use a rubber

band or similar). See that the substance is close to
the bulb as shown in the enlargement in the picture
on the side of the page.

14- Next fix the apparatus as shown in the picture. The

liquid in the beaker is water but it is better to use
mineral oil.

15- Heat strongly until the thermometer reaches 65 –

70°C.

16- Now heat very slowly so the temperature rises at a

rate of just one or two degrees per minute (very
slowly).

17- Keep an eye always on the sample (if you have a

magnifying glass it will help) and as soon as it starts
melting stop heating.

18- Record this temperature and the temperature at which the naphthalene is totally
molten.

19- Does it agree with the expected value? What can you say about the purity before and
after sublimation?