28: Dehydration of sucrose and a version of pharaohs

serpent.
Demonstration 1: This can be a spectacular demonstration and is often used to show
the very high affinity of concentrated sulfuric acid for water in that it can remove the
elements of water from a carbohydrate such as sucrose (table sugar).
C12H22O11 - 11H2O

12C

However, it seems that the reaction is not quite that direct. If concentrated sulfuric
acid is added to a layer of sugar in a Pyrex beaker the sugar turns brown but usually
there is no violent reaction. To get a spectacular column of aerated carbon particles
that often reaches beyond the top of the beaker it seems necessary to first add water to
the sugar and then pour in the sulfuric acid slowly. It seems that the high temperature
generated by the reaction between the acid and the water is sufficient to cause the
following reaction to occur:
C12H22O11

11H2O + 12C

This is, of course EXACTLY equivalent to the first equation, but this reaction is itself
slightly exothermic, and does not occur readily with dry sugar and concentrated
sulfuric acid.
Cover the base of a Pyrex beaker (250cm3) with about 1cm depth of granular table
sugar. Pour in sufficient distilled water to just reach the top surface of the sugar
granules. Taking great care gently pour in concentrated sulfuric acid until the liquid
begins to boil. The boiling usually spreads to cover the whole surface of the sugar and
a black foam of finely divided carbon rises in the beaker often reaching well beyond
the rim of the beaker.
The reaction is accompanied by the smell of toffee/caramel although tainted with
sulfur dioxide. It should be carried out on a fume cupboard. (See final section for
safety advice.)
Demonstration 2: A second method of dehydrating sucrose that does not use
concentrated sulfuric acid is to use an oxidising agent with a substantial excess of
sugar. The oxidation of some of the sucrose produces sufficient heat to raise the
temperature such that dehydration of the remaining sucrose will occur. In some ways
this reaction which results in an extended mass of very finely divided carbon
resembles a classical demonstration of the pharaohs serpent. (A serpent-like mass of
resulting from the burning / decomposition of a pellet the serpents egg made from
mercury II thiocyanate this reaction uses and produces highly toxic materials and
could not be recommended for use nowadays.) There are many recipes to be found on
the internet to make a so-called black snake or serpent and that given below is based
on a suggestion from the University of Minnesota
(www.chem.umn.edu/services/lecturedemo/info/sugar_dehydration.html) (accessed
June 2011). The heat generated by the oxidation of a small proportion (about 16%) of

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the sugar is sufficient to provide the activation energy for the dehydration of the rest
as shown by the equation in the previous section.

Carefully cut the nozzle end from a disposable plastic syringe (Somewhere
between 25 and 60mL seems to be a suitable size) to create a suitable mould to
form a serpents egg

Grind separately in a pestle and mortar 15g of table sugar (sucrose) and 4g of
potassium chlorate. Carefully mix these two powders intimately being aware
that this is a potentially explosive mixture so mixing with a wooden spatula is
preferred to even light grinding in a mortar with a pestle.

Pull back the plunger of the syringe to about the 20mL mark and add sufficient
of the powder mixture to produce a layer about 1cm in depth. Add sufficient
ethanol (methylated spirits) to the syringe to thoroughly wet the powder and
tap the plunger lightly to remove air bubbles.

Repeat the addition of powder and methylated spirits until the powder is used.

Cover the open end of the syringe with a piece of scrap metal or the base of a
metal dish and depress the plunger firmly on to the metal to compress the
plug of powder soaked in methylated spirits.

Very carefully invert the syringe on to the surface of a metal tray on which the
reaction can occur (ensure the surface under the tray is sufficiently protected
from the considerable heat generated when the reaction occurs) and slowly
push the plug out onto the surface. The smaller the diameter of the syringe the
taller will be the egg and the more care needs to be taken to avoid the egg
breaking up as it is laid!

Ensure there is no inflammable material within 1m and ignite the plug with a
match or lighted taper. Initially the methylated spirits burn quietly before
igniting the reaction mixture. As the black foam emerges it looks vaguely
living (from a horror movie) and some spitting may occur.

Wait until the resulting mass of carbon (with KCl) and metal tray have cooled
before attempting to clear up.

Education issues:
Usually done to show the strong affinity between sulfuric and water although as
discussed above the connection is perhaps not quite as direct as is often implied.
The second reaction seems to demonstrate pyrotechnic applications rather than direct
chemical principles although a creative teacher may find a number of reasons to show
the demonstration. It would certainly provide an interesting event at a science fair or a
parents evening.
Risk assessment: (You MUST make your own)
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Demonstration 1: Concentrated sulfuric acid is a dangerous liquid that is a strong

oxidising agent (it produces sulfur dioxide when it acts this way) and reacts violently
with water to form a strongly acidic solution. Eye protection must be worn and care
taken not to get the acid on the skin. (Should this happen, wipe off as much of the acid
ac possible with a dry cloth any piece of clothing and rinse immediately with large
amounts of water. (It is important not to dilute large amounts of the acid whilst in
contact with skin since temperatures well over 150oC can be generated and cause
additional serious burns. For this reason and substantial amount of concentrated acid
in the eye or mouth would be very serious and require medical attention.)
The beaker should be placed inside a larger beaker or on an acid-proof tray to contain
any spillage should the beaker break due to the thermal shock. (This should not
happen but may do if the beaker has and deep scratches or small cracks.)
The remaining mass of carbon remains very hot for some time it also contains
substantial amounts of sulfuric acid. When cold it can be placed under a running water
tap when the diluted acid and much of the carbon powder is flushed down the sink. It
may be difficult to remove all the carbon residue from the beaker in which case it may
be useful to dry the beaker and reserve it for any repeat runs of this demonstration.
Demonstration 2: The main potential hazard has already been mentioned since
vigorous mixing of the mixture can conceivably cause the reaction to begin. It is very
unlikely to happen (and I have never managed to start the reaction this way even
when I have tried.) It is nevertheless wise to take precautions.
The reaction produces flame and sparks and eye protection and a safety screen should
be used. There are no hazardous by-products and the reaction can be carried out in a
well ventilated room. Wait until all has cooled sufficiently before attempting to move
the tray or clear up.

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