=155. Method Of Krug.=—In conducting the determination of furfurol,
according to the method of Chalmont and Tollens just noticed, Krug
observed that the filtrate, after standing for some time, yielded a
second precipitate of furfurol hydrazone. Great difficulty was also
experienced in collecting the precipitate upon the filter on account
of the persistency with which it stuck to the sides of the vessel
in which the precipitation took place.[129] In order to avoid these
two objections, Krug modified the method as described below and this
modified method is now exclusively used in this laboratory.
After the precipitation of the furfurol hydrazone, it is stirred
vigorously, by means of an appropriate mechanical stirrer, for at
least half an hour and then allowed to rest for twenty-four hours. On
filtering after that length of time the filtrate remains perfectly
clear and no further precipitation takes place. After the filtration is
complete and the beaker and filtering tube well washed, no attempt is
made to detach the part of the filtrate adhering to the beaker but the
whole of the precipitate, both that upon the filter and that adhering
to the sides of the beaker, is dissolved in strong alcohol, from thirty
to forty cubic centimeters being used. The alcoholic solution is
collected in a small weighed flask, the alcohol evaporated at a gentle
heat and the last traces of water removed by heating to 60° and blowing
a current of dry air through the flask. After weighing the precipitate
of furfurol hydrazone, obtained as above, the calculation of the weight
of pentose bodies is accomplished by means of the usual factors.
=156. Precipitation of Furfurol with Pyrogalol.=—Furfurol is thrown
out of solution in combination with certain phenol bodies by heating
together in an acid solution. Hotter has proposed a method for the
determination of furfurol based on the above fact.[130] The furfurol
is obtained by distillation in the manner already described and
hydrochloric acid is added if necessary to secure twelve per cent of
that body in a given volume. The furfurol is thrown out of an aliquot
portion by heating with an excess of pyrogalol in closed tubes for
about two hours at 110°. The reaction takes place in two stages,
represented by the following equations:
C₅H₄O₂ + C₆H₆O₃ = C₁₁H₁₀O₅
and
2C₁₁H₁₀O₅ = C₂₂H₁₈O₉ + H₂O.
The aliquot part of the distillate used should not contain more than
one-tenth of a gram of furfurol. The precipitate formed in this way is
collected on an asbestos felt, dried at 103° and weighed. The weight
obtained divided by 1.974 gives the corresponding amount of furfurol.
There is some difficulty experienced in loosening the precipitate from
the sides of the tubes in which the heating takes place, but this
defect can be overcome by heating in covered beakers in an autoclave.
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