=181. Separation by Hydrolysis with Water at High
Temperatures.=—Instead of dissolving the starch with diastase, it may
be brought into solution by heating with water under pressure. The
former method employed of heating in sealed flasks has been entirely
superceded by heating in an autoclave. The materials are best held in
metal beakers furnished with a cover which prevents loss from boiling
if the pressure should be removed too rapidly after the completion
of the operation. The autoclave is a strong metal vessel capable of
resisting the pressure of several atmospheres. It is furnished with a
pressure gauge C and a safety valve D, as shown in the figure. The top
is securely screwed on by means of a wrench, shown at the right hand
side. In the figure a portion of the case is represented cut away to
show the arrangement of the metal beakers inside.
In the method of Reinke, as practiced at the Halle station, and in
this laboratory, about three grams of the starchy substance are placed
in each of the metal beakers with twenty-five cubic centimeters of
a one per cent lactic acid solution and thirty cubic centimeters of
water. The contents of the beaker are thoroughly mixed and they are
then heated for two and a half hours in the autoclave, at a pressure
of three and a half atmospheres. The addition of the lactic acid is
for the purpose of protecting any sugar which may be present from
decomposition at the high pressure and temperature employed. After
the completion of the heating, the autoclave is allowed to cool, the
cover is removed and the beakers taken out and their contents washed
with hot water into quarter liter flasks. After cooling, the volume
is completed with cold water, and after standing for half an hour,
with frequent shaking, the contents of the flasks are filtered and
200 cubic centimeters of the filtrate in each case converted into
dextrose with hydrochloric acid in the usual way. In order to obtain
agreeing results, it is highly necessary that the substance before
treatment should be ground to a fine powder. The addition of the lactic
acid, as practiced in the reinke method, tends to give somewhat high
results, due probably to the hydrolytic action of the acid on the
fiber present. When starchy bodies are heated in the autoclave for the
determination of their starch by polarimetric methods, or for ordinary
determinations, the use of lactic acid should be omitted.
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