=150. Estimation of Pentose Sugars and Pentosans as Furfurol.=—The
production of furfurol by distilling carbohydrates with an acid has
already been mentioned. Tollens and his associates have shown that with
pentose sugars, and carbohydrate bodies yielding them, the production
of furfurol is quantitive.
The production and estimation of furfurol have been systematically
studied by Krug, to whose paper the reader is referred for the complete
literature of the subject.[123] The essential principles of the
operation are based on the conversion of the pentoses into furfurol by
distilling with a strong acid, and the subsequent precipitation and
estimation of the furfurol formed in the first part of the reaction.
The best method of conducting the distillation is as follows:
Five grams of the pentose substance are placed in a flask of about a
quarter liter capacity, with 100 cubic centimeters of hydrochloric acid
of 1.06 specific gravity. The arrangement of the apparatus is shown in
Fig. 46. The flame of the lamp is so regulated as to secure about two
cubic centimeters of distillate per minute.
[Illustration: FIGURE 46. DISTILLING APPARATUS FOR PENTOSES.]
The distillate is received in a graduated cylinder and as soon
as thirty cubic centimeters are collected, an equal quantity of
hydrochloric acid, of the strength noted, is added to the distilling
flask, allowing it to flow in slowly so as not to stop the ebullition.
The process is continued until a drop of the distillate gives no
sensible reaction for furfurol when tested with anilin acetate. The
test is applied as follows: Place a drop of the distillate on a piece
of filter paper moistened with anilin acetate. The presence of furfurol
will be disclosed by the production of a brilliant red color. Usually
about three hours are consumed in the distillation, during which time a
little less than 400 cubic centimeters of distillate is obtained. The
distillate is neutralized with solid sodium carbonate and, in order
to have always the same quantity of common salt present, 10.2 grams
of sodium chlorid are added for each fifty cubic centimeters of water
necessary to make the total volume to half a liter.[124]
The reactions with pentosans probably consist in first splitting up of
the molecule into a pentose and the subsequent conversion of the latter
into furfurol according to the following equations:
(C₅H₈O₄)ₙ + (H₂O)ₙ = (C₅H₁₀O₅)ₙ
Pentosan. Water. Pentose.
and
(C₅H₁₀O₅)ₙ = (C₅H₄O₂)ₙ + (3H₂O)ₙ.
Pentose. Furfurol. Water.
=151. Determination of Furfurol.=—The quantity of furfurol obtained by
the process mentioned above may be determined in several ways.
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