(6) Bulbed =U= tubes or Will’s bulbs, as described under the soda-lime
method:
_Manipulation._—(a) Clean the =U= tube and introduce ten cubic
centimeters of standard acid.
(b) Fit the cork and glass connecting tube. Fill the tube as follows:
(1) A loosely fitting plug of asbestos, previously ignited, and then
two and five-tenths to three and five-tenths centimeters of the
thiosulfate mixture: (2) The weighed portion of the substance to
be analyzed is intimately mixed with from five to ten grams of the
sugar and sulfur mixture: (3) Pour on a piece of glazed paper or in
a porcelain mortar a sufficient quantity of thiosulfate mixture to
fill about twenty-five centimeters of the tube; then add the substance
to be analyzed, as previously prepared, mix carefully, and pour into
the tube; shake down the contents of the tube; rinse off the paper or
mortar with a small quantity of the thiosulfate mixture and pour into
the tube; then fill up with soda-lime to within five centimeters of the
end of the tube: (4) Place another plug of ignited asbestos at the end
of the tube and close with a cork: (5) Hold the tube in a horizontal
position and tap on the table until there is a gas-channel along the
top of the tube: (6) Make connection with the =U= tube containing the
acid; aspirate and see that the apparatus is tight.
_The Combustion._—Place the prepared combustion tube in the furnace,
letting the open end project a little, so as not to burn the cork.
Commence by heating the soda-lime portion until it is brought to a full
red heat. Then turn on slowly jet after jet toward the outer end of
the tube, so that the bubbles come off two or three a second. When the
whole tube is red hot and the evolution of the gas has ceased and the
liquid in the =U= tube begins to recede toward the furnace, attach the
aspirator to the other limb of the =U= tube, break off the end of the
tube, and draw a current of air through for a few minutes. Detach the
=U= tube and wash the contents into a beaker or porcelain dish; add a
few drops of the cochineal solution, and titrate.
=176. Observations.=—In our experience we have found it much more
satisfactory to adhere to the earlier directions for preparing the
mixture of thiosulfate and alkali. We much prefer to make the mixture
with soda-lime and without the previous drying of the sodium salt.
Ruffle himself says that the sodium thiosulfate should be dry but not
deprived of its water of crystallization.[146] The best method to dry
the crystal powder without depriving it of its crystal water is to
press it between blotting papers. The official method also contains
a typographical error in prescribing that the combustion tube should
have a length of thirty centimeters where evidently thirty inches were
meant. Ruffle’s original tube was twenty-two inches in length.
Public-domain text, read in full here on John Shaqi.
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