starch in a cereal or similar substance can be completed within two
hours. The chief amount of time saved is in the heating with the malt
extract, which instead of being continued for two hours, as usually
directed, can be accomplished in thirty minutes.[159]
=192. Precipitation of Starch with Barium Hydroxid.=—The tendency of
carbohydrate bodies to unite with the earthy bases has been utilized by
Asboth as a basis for the quantitive determination of starch.[160]
About three grams of the finely ground sample containing the starch,
or one gram of pure starch, are rubbed up in a mortar with water and
the detached starch remaining suspended in the wash water is poured
off. This operation is repeated until all the starch is removed. In
difficult cases hot water may be used. The starch thus separated is
heated in a quarter liter flask to the boiling point to reduce it to
the condition of paste. When the paste is cold it is treated with fifty
cubic centimeters of the barium hydroxid solution, the flask closed and
well shaken for two minutes. The volume is then completed to the mark
with forty-five per cent alcohol, the flask well shaken and allowed
to stand. In a short time the barium-starch compound separates and
settles. Fifty cubic centimeters of the clear supernatant liquor are
removed with a pipette, or the liquor may be passed through a filter
and the quantity mentioned removed for titration of the residual barium
hydroxid after the addition of a few drops of phenolphthalein solution.
The quantity of barium hydroxid remaining, deducted from the original
quantity, gives the amount which has entered into composition with
the starch; the composition of the molecule being BaOC₂₄H₄₀O₂₀, which
contains 19.10 per cent of barium oxid and 80.90 per cent of starch.
The set solution of barium hydroxid must be preserved from contact with
the carbon dioxid of the air. The burette should be directly attached
to the bottle holding the set solution, by any of the usual appliances,
and the air entering the bottle must be deprived of carbon dioxid. The
water used in the work must be also free of air, and this is secured by
boiling immediately before use.
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