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.
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.
_Standard thermometer_ graduated in tenths of a degree.
DETERMINATION--The sample should be clear when melted and entirely free from moisture, or incorrect results will be obtained.
Melt and thoroughly mix the sample. Dip three of the capillary tubes above described in the oil so that the fat in the tube stands about 1 cm. in height. Now fuse the capillary end carefully by means of a small blast flame and allow to cool. These tubes are placed in a refrigerator over night at a temperature of from 40 to 50° F. They are then fastened by means of a rubber band or other suitable means to the bulb of a thermometer graduated in tenths of a degree. The thermometer is suspended in a beaker of water (which is agitated by air or other suitable means) so that the bottom of the bulb of the thermometer is immersed to a depth of about 3 cm. The temperature of the water is increased gradually at the rate of about 1° per minute.