Ascagne Sobrero, the discoverer of Nitro-Glycerin, says: it may be
prepared by slowly introducing syrupy Glycerin into a mixture of two
volumes concentrated sulphuric acid to one volume of nitric acid, Sp.
Gr. 1.4, dropping it in and rapidly cooling. It seems to dissolve in
this mixture without any noticeable reaction, and by pouring it into
water, the so formed Nitro-Glycerin separates from it. It is then
washed several times in water, is next dissolved in ether, and after
evaporation (dangerous work this) is finally purified over sulphuric
acid.
De Vrij recommends dissolving 100 grammes of Glycerin Sp. Gr. 1.262 in
200 c. c. of hydrated nitric acid cooled to 14°F, taking care that the
mixture never exceeds in temperature 32°F. When a homogeneous mixture
has been obtained, 200 c. c. of strong sulphuric acid are added very
gradually, taking especial care that the temperature of this mixture
never rises above 32°F. The oily Nitro-Glycerin which floats on the
surface is separated by a tap-funnel from the acid liquid (which
yields more Nitro-Glycerin on being diluted with water) and is now
dissolved in the smallest possible quantity of ether; this solution
is shaken with water, until the water no longer reddens litmus; the
ether evaporated (here take care!) and the remaining Nitro-Glycerin
heated over the water-bath till its weight remains constant. Merck,
of Darmstadt, the eminent operative chemist, found in following De
Vrij’s method, whilst evaporating the ethereal solution, and before
the temperature had reached 212°F, it was accompanied by a terrible
explosion. An accident from the same cause occurred in the laboratory
of Dr. E. Von Gorup-Besanez, and we find in “Comptes Rendus” an account
of the effects of the explosion of only 10 drops of Nitro-Glycerin,
which, by one of the pupils of that chemist, in his laboratory, were
put into a small cast-iron saucepan, and heated with a Bunsen gas
flame. The effect of the explosion was that the forty-six panes of
glass of the windows of the laboratory were smashed to atoms, the
saucepan was hurled through a brick wall, the stout iron stand on which
the vessel had been placed was partly split, partly spirally twisted,
and the tube of the Bunsen burner was split and flattened outwards.
Fortunately, none of the three persons present in the laboratory at the
time were hurt. When Nitro-Glycerin is caused to fall drop by drop on a
thoroughly red hot iron plate, it burns off as gunpowder would do under
the same conditions; but if the iron is not red hot, but yet hot enough
to cause the Nitro-Glycerin to boil suddenly, an explosion takes place.
Nitro-Glycerin is decomposed by evaporation, even in vacuo, over
sulphuric acid at ordinary temperatures (RAILTON), and when left to
itself, frequently undergoes spontaneous decomposition; but when well
purified, it may be kept for a long time without alteration (H. WATTS);
exhibits different properties, according to the manner in which it is
prepared (GLADSTONE).
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