Principles and practice of agricultural analysis. Volume 3 (of 3), Agricultural products

by Harvey Washington Wiley

The melted fat or fat acid is placed in a test tube contained in a large bottle, which serves as a jacket to protect the tube from sudden or violent changes of temperature. The efficiency of the jacket may be increased by exhausting the air therefrom, as in the apparatus for determining the heat of bromination, hereafter described. A very delicate thermometer, graduated in tenths of a degree, and having a long bulb, is employed. By means of the reading glass, the reading can be made in twentieths of a degree. The arrangement of the apparatus is shown in [Fig. 85]. The test tube is nearly filled with the melted matter. The bottom of the jacket should be gently warmed to prevent a too rapid congelation in the bottom of the test tube containing the melted fat, and the tube is to be so placed as to leave an air space between it and the bottom of the bottle. The thermometer is suspended in such a manner as to have the bulb as nearly as possible in the center of the melted fat. The thermometer should be protected from air currents and should be kept perfectly still. In case the congealing point is lower than room temperature the jacket may be immersed in a cooling mixture, the temperature of which is only slightly below the freezing point of the fatty mass.

When crystals of fat begin to form, the descent of the mercury in the stem of the thermometer will become very slow and finally reach a minimum, which should be noted. As the crystallization extends inwards and approaches the bulb of the thermometer a point will be reached when the mercury begins to rise. At this time the partially crystallized mass should be vigorously stirred with the thermometer and again left at rest in as nearly, the original position as possible. By this operation the mercury will be made to rise and its maximum position should be noted as the true crystallizing point of the whole mass. In comparing different samples, it is important that the elements of time in which the first crystallization takes place should be kept, as nearly as possible, the same. A unit of one hour in cooling the mixture from a temperature just above its point of fusion until the incipient crystallization is noticed, is a convenient one for glycerids and for fat acids.

294. Determination of Refractive Power.—The property of refracting light is possessed by fats in different degrees and these differences are of great help in analytical work. The examination may be made by the simple refractometer of Abbe or Bertrand, or by the more elaborate apparatus of Pulfrich.

The comparative refractive power of fats can also be observed by means of the oleorefractometer of Amagat-Jean or the differential refractometer of Zune.[247]

For details of the construction of these apparatus, with a description of the optical principles on which they are based, the papers above cited may be consulted. In this laboratory the instruments which have been employed are three in number, viz., Abbe’s small refractometer, Pulfrich’s refractometer using yellow light, and the oleorefractometer of Amagat-Jean. A brief description of the methods of manipulating these instruments is all that can be attempted in this manual.

295. Refractive Index.—Refractive index is an expression employed to characterize the measurement of the degree of deflection caused in a ray of light in passing from one transparent medium into another. It is the quotient of the sine of the angle of the incident, divided by the sine of the angle of the refracted ray.

In the case of oils which remain liquid at room temperatures, the determinations can be made without the aid of any device to maintain liquidity. In the case of fat which becomes solid at ordinary room temperatures, the determination must either be made in a room artificially warmed or the apparatus must have some device, as in the later instruments of Abbe and Pulfrich, and in the apparatus of Amagat-Jean, whereby the sample under examination can be maintained in a transparent condition. In each case the accuracy of the apparatus should be tested by pure water, the refractive index of which at 18° is 1.333. The refractive index is either read directly on the scale as in Abbe’s instrument, or calculated from the angles measured as in Pulfrich’s apparatus.

Fig. 86.—Abbe’s Refractometer.

296. Abbe’s Refractometer.—For practical use the small instrument invented by Abbe will be found sufficient. The one which has been in use for many years in this laboratory is shown in [Fig. 86]. The illustration represents the apparatus in the position preliminary to reading the index. In preparing the sample of oil for observation the instrument is turned on its axis until the prisms between which the oil is placed assume a horizontal position, as is seen in [Fig. 87]. The movable prism is unfastened and laid aside, the fixed prism covered with a rectangular shaped piece of tissue paper on which one or two drops of the oil are placed. The movable prism is replaced in such a manner as to secure a complete separation of the two prisms by the film of oiled tissue paper. A little practice will enable the analyst to secure this result.