The titer of a fat or oil is really an indication of the amount of stearic acid contained therein. The titer, expressed in degrees Centigrade, is the solidification point of the fatty acids of an oil or fat. In order to carry out the operation a Centigrade thermometer graduated in one or two-tenths of a degree is necessary. A thermometer graduated between 10 degs. centigrade to 60 degs. centigrade is best adapted and the graduations should be clear cut and distinct.
To make the determination about 30 grams of fat are roughly weighed in a metal dish and 30-40 cubic centimeters of a 30 per cent. (36 degs. Baumé) solution of sodium hydroxide, together with 30-40 cubic centimeters of alcohol, denatured alcohol will do, are added and the mass heated until saponified. Heat over a low flame or over an asbestos plate until the soap thus formed is dry, constantly stirring the contents of the dish to prevent burning. The dried soap is then dissolved in about 1000 cubic centimeters of water, being certain that all the alcohol has been expelled by boiling the soap solution for about half an hour. When the soap is in solution add sufficient sulphuric acid to decompose the soap, approximately 100 cubic centimeters of 25 degs. Baumé sulphuric acid, and boil until the fatty acids form a clear layer on top of the liquid. A few pieces of pumice stone put into the mixture will prevent the bumping caused by boiling. Siphon off the water from the bottom of the dish and wash the fatty acids with boiling water until free from sulphuric acid. Collect the fatty acids in a small casserole or beaker and dry them over a steam bath or drying oven at 110 degs. Centigrade. When the fatty acids are dry, cool them to about 10 degs. above the titer expected and transfer them to a titer tube or short test tube which is firmly supported by a cork in the opening of a salt mouth bottle. Hang the thermometer by a cord from above the supported tube so it reaches close to the bottom when in the titer tube containing the fatty acids and so that it may be used as a stirrer. Stir the mass rather slowly, closely noting the temperature. The temperature will gradually fall during the stirring operation and finally remain stationary for half a minute or so then rise from 0.1 to 0.5 degs. The highest point to which the mercury rises after having been stationary is taken as the reading of the titer.
DETERMINATION OF UNSAPONIFIABLE MATTER.
In order to determine the unsaponifiable matter in fats and oils they are first saponified, then the unsaponifiable, which consists mainly of hydrocarbons and the higher alcohols cholesterol or phytosterol, is extracted with ether or petroleum ether, the ether evaporated and the residue weighed as unsaponifiable.
To carry out the process first saponify about 5 grams of fat or oil with an excess of alcoholic potassium hydrate, 20-30 cubic centimeters of a 1 to 10 solution of potassium hydroxide in alcohol until the alcohol is evaporated over a steam bath. Wash the soap thus formed into a separatory funnel of 200 cubic centimeters capacity with 80-100 cubic centimeters water. Then add about 60 cubic centimeters of ether, petroleum ether or 86 degs. gasoline and thoroughly shake the funnel to extract the unsaponifiable. Should the two layers not separate readily, add a few cubic centimeters of alcohol, which will readily cause them to separate. Draw off the watery solution from beneath and wash the ether with water containing a few drops of sodium hydrate and run to another dish. Pour the watery solution into the funnel again and repeat the extraction once or twice more or until the ether shows no discoloration. Combine the ether extractions into the funnel and wash with water until no alkaline reaction is obtained from the wash water. Run the ether extract to a weighed dish, evaporate and dry rapidly in a drying oven. As some of the hydrocarbons are readily volatile at 100 degs. Centigrade, the drying should not be carried on any longer than necessary. The residue is then weighed and the original weight of fat taken divided into the weight of the residue × 100 gives the percentage unsaponifiable.
TEST FOR COLOR OF SOAP.
It is often desirable to determine the color of the finished soap by a rapid determination before it is made into soap. It often happens, especially with the tallows, that a dark colored sample produces a light colored soap, whereas a bleached light colored tallow produces a soap off shade.
To rapidly determine whether the color easily washes out of the tallow with lye, 100 cubic centimeters of tallow are saponified in an enameled or iron dish with 100 cubic centimeters of 21 degs. Baumé soda lye and 100 cubic centimeters of denatured alcohol. Continue heating over a wire gauze until all the alcohol is expelled and then add 50 cubic centimeters of the 21 degs. Baumé lye to grain the soap. Allow the lyes to settle and with an inverted pipette draw off the lyes into a test tube or bottle. Close the soap with 100 cubic centimeters of hot water and when closed again grain with 50 cubic centimeters of the lye by just bringing to a boil over an open flame. Again allow the lyes to settle and put aside a sample of the lye for comparison. Repeat the process of closing, graining and settling and take a sample of lye. If the lye is still discolored repeat the above operations again or until the lye is colorless. Ordinarily all the color will come out with the third lye. The soap thus obtained contains considerable water which makes it appear white. The soap is, therefore, dried to about 15 per cent. moisture and examined for color. The color thus obtained is a very good criterion as to what may be expected in the soap kettle.
By making the above analyses of fats or oils the main properties as to their adaptability for being made into soap are determined. In some cases, especially where adulteration or mixtures of oils are suspected, it is necessary to further analyze same. The methods of carrying out these analyses are fully covered by various texts on fats and oils and we will not go into details regarding the method of procedure in carrying these out.