was used to liberate the
iodine when it was prepared. It may be purified by sublimation after
mixing it with a little potassium iodide, which reacts with the iodine
chloride, forming potassium chloride and setting free the iodine. The
sublimed iodine is then dried by placing it in a closed container over
concentrated sulphuric acid. It may then be weighed in a stoppered
weighing-tube and dissolved in a solution of potassium iodide in a
stoppered flask to prevent loss of iodine by volatilization. About 18
grams of the iodide and twelve grams of iodine per liter are required
for an approximately tenth-normal solution.
An iodine solution made from commercial iodine may also be
standardized against arsenious oxide (As_{4}O_{6}). This substance
also usually requires purification by sublimation before use.
The substances usually employed for the standardization of a
thiosulphate solution are potassium bromate and metallic copper. The
former is obtainable in pure condition or may be easily purified by
re-crystallization. Copper wire of high grade is sufficiently pure
to serve as a standard. Both potassium bromate and cupric salts in
solution will liberate iodine from an iodide, which is then titrated
with the thiosulphate solution.
The reactions involved are the following:
(a) KBrO_{3} + 6KI + 3H_{2}SO_{4} --> KBr + 3I_{2} + 3K_{2}SO_{4} + 3H_{2}O,
(b) 3Cu + 8HNO_{3} --> 3Cu(NO_{3})_{2} + 2NO + 4H_{2}O,
2Cu(NO_{3})_{2} + 4KI --> 2CuI + 4KNO_{3} + I_{2}.
Two methods for the direct standardization of the sodium thiosulphate
solution are here described, and one for the direct standardization of
the iodine solution.
!Method A!
PROCEDURE.--Weigh out into 500 cc. beakers two portions of about
0.150-0.175 gram of potassium bromate. Dissolve each of these in 50
cc. of water, and add 10 cc. of a potassium iodide solution containing
3 grams of the salt in that volume (Note 1). Add to the mixture 10 cc.
of dilute sulphuric acid (1 volume of sulphuric acid with 5 volumes of
water), allow the solution to stand for three minutes, and dilute to
150 cc. (Note 2). Run in thiosulphate solution from a burette until
the color of the liberated iodine is nearly destroyed, and then add 1
cc. or 2 cc. of starch solution, titrate to the disappearance of the
iodo-starch blue, and finally add iodine solution until the color
is just restored. Make a blank test for the amount of thiosulphate
solution required to react with the iodi
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