Standardization of the Sodium Thiosulfate Solution—Place 40 cc. of the potassium bichromate solution, to which has been added 10 cc. of the solution of potassium iodide, in a glass-stoppered flask. Add to this 5 cc. of strong hydro-chloric acid. Dilute with 100 cc. of water, and allow the N/10 sodium thiosulfate to flow slowly into the flask until the yellow color of the liquid has almost disappeared. Add a few drops of the starch paste, and with constant shaking continue to add the N/10 sodium thiosulfate solution until the blue color just disappears.
Determination—Weigh accurately from 0.10 to 0.50 g. (depending on the iodine number) of the melted and filtered sample into a clean, dry, 16-oz. glass-stoppered bottle containing 15-20 cc. of carbon tetrachloride or chloroform. Add 25 cc. of iodine solution from a pipette, allowing to drain for a definite time. The excess of iodine should be from 50 per cent to 60 per cent of the amount added, that is, from 100 per cent to 150 per cent of the amount absorbed. Moisten the stopper with a 15 per cent potassium iodide solution to prevent loss of iodine or chlorine but guard against an amount sufficient to run down inside the bottle. Let the bottle stand in a dark place for 1/2 hr. at a uniform temperature. At the end of that time add 20 cc. of 15 per cent potassium iodide solution and 100 cc. of distilled water. Titrate the iodine with N/10 sodium thiosulfate solution which is added gradually, with constant shaking, until the yellow color of the solution has almost disappeared. Add a few drops of starch paste and continue titration until the blue color has entirely disappeared. Toward the end of the reaction stopper the bottle and shake violently so that any iodine remaining in solution in the tetrachloride or chloroform may be taken up by the potassium iodide solution. Conduct two determinations on blanks which must be run in the same manner as the sample except that no fat is used in the blanks. Slight variations in temperature quite appreciably affect the titer of the iodine solution, as acetic acid has a high coefficient of expansion. It is, therefore, essential that the blanks and determinations on the sample be made at the same time. The number of cc. of standard thiosulfate solution required by the blank, less the amount used in the determination, gives the thiosulfate equivalent of the iodine absorbed by the amount of sample used in the determination. Calculate to centigrams of iodine absorbed by 1 g. of sample (= per cent iodine absorbed).
Determination, Tung Oil—Tung oil shows an erratic behavior with most iodine reagents and this is particularly noticeable in the case of the Hanus reagent which is entirely unsuitable for determining the iodine number of this oil since extremely high and irregular results are obtained. The Hübl solution shows a progressive absorption up to 24 hrs. and probably for a longer time but the period required is entirely too long for a chemical determination. The Wijs solution gives good results if the following precautions are observed:
Weigh out 0.15 ± 0.05 g., use an excess of 55 ± 3 per cent Wijs solution. Conduct the absorption at a temperature of 20-25° C. for 1 hr. In other respects follow the instructions detailed above.
SAPONIFICATION NUMBER (KOETTSTORFER NUMBER).
Preparation of Reagents. N/2 Hydrochloric Acid—Carefully standardized.
Alcoholic Potassium Hydroxide Solution—Dissolve 40 g. of pure potassium hydroxide in one liter of 95 per cent redistilled alcohol (by volume). The alcohol should be redistilled from potassium hydroxide over which it has been standing for some time, or with which it has been boiled for some time, using a reflux condenser. The solution must be clear and the potassium hydroxide free from carbonates.
Determination—Weigh accurate about 5 g. of the filtered sample into a 250 to 300 cc. Erlenmeyer flask. Pipette 50 cc. of the alcoholic potassium hydroxide solution into the flask, allowing the pipette to drain for a definite time. Connect the flask with an air condenser and boil until the fat is completely saponified (about 30 minutes). Cool and titrate with the N/2 hydrochloric acid, using phenolphthalein as an indicator. Calculate the Koettstorfer number (mg. of potassium hydroxide required to saponify 1 g. of fat). Conduct 2 or 3 blank determinations, using the same pipette and draining for the same length of time as above.
MELTING POINT.
Apparatus—Capillary tubes made from 5 mm. inside diameter thin-walled glass tubing drawn out to 1 mm. inside diameter. Length of capillary part of tubes to be about 5 cm. Length of tube over all 8 cm.