From the data obtained, calculate the relation of the thiosulphate solution to a normal solution, and subsequently calculate the similar value for the iodine solution.

[Note 1:—­Potassium iodide usually contains small amounts of potassium iodate as impurity which, when the iodide is brought into an acid solution, liberates iodine, just as does the potassium bromate used as a standard.  It is necessary to determine the amount of thiosulphate which reacts with the iodine thus liberated by making a “blank test” with the iodide and acid alone.  As the iodate is not always uniformly distributed throughout the iodide, it is better to make up a sufficient volume of a solution of the iodide for the purposes of the work in hand, and to make the blank test by using the same volume of the iodide solution as is added in the standardizing process.  The iodide solution should contain about 3 grams of the salt in 10 cc.]

[Note 2:  The color of the iodo-starch is somewhat less satisfactory in concentrated solutions of the alkali salts, notably the iodides.  The dilution prescribed obviates this difficulty.]

!Method B!

Procedure.—­Weigh out two portions of 0.25-0.27 gram of clean copper wire into 250 cc.  Erlenmeyer flasks (Note 1).  Add to each 5 cc. of concentrated nitric acid (sp. gr. 1.42) and 25 cc. of water, cover, and warm until solution is complete.  Add 5 cc. of bromine water and boil until the excess of bromine is expelled.  Cool, and add strong ammonia (sp. gr. 0.90) drop by drop until a deep blue color indicates the presence of an excess.  Boil the solution until the deep blue is replaced by a light bluish green, or a brown stain appears on the sides of the flask (Note 2).  Add 10 cc. of strong acetic acid (sp. gr. 1.04), cool under the water tap, and add a solution of potassium iodide (Note 3) containing about 3 grams of the salt, and titrate with thiosulphate solution until the color of the liberated iodine is nearly destroyed.  Then add 1-2 cc. of freshly prepared starch solution, and add thiosulphate solution, drop by drop, until the blue color is discharged.

From the data obtained, including the “blank test” of the iodide, calculate the relation of the thiosulphate solution to the normal.

[Note 1:  While copper wire of commerce is not absolutely pure, the requirements for its use as a conductor of electricity are such that the impurities constitute only a few hundredths of one per cent and are negligible for analytical purposes.]

[Note 2:  Ammonia neutralizes the free nitric acid.  It should be added in slight excess only, since the excess must be removed by boiling, which is tedious.  If too much ammonia is present when acetic acid is added, the resulting ammonium acetate is hydrolyzed, and the ammonium hydroxide reacts with the iodine set free.]

[Note 3:  A considerable excess of potassium iodide is necessary for the prompt liberation of iodine.  While a large excess will do no harm, the cost of this reagent is so great that waste should be avoided.]