Determination of Titer Value of Oils, Wax and Fat

This testing method determines the solidification point of the fatty acid like Soap, Oil, Fat, Wax, etc. This test method applies to fatty acids.

Apparatus

For titer above 35 °C. Griffin low-form beaker, 2-liter capacity and wide mouth bottle, capacity 450 ml, height 190 mm, and inside diameter of neck 38 mm. Assemble as shown in the below image.

A glass beaker may be used instead of stainless steel if it is desired to observe the sample during the test. In this case, the 5800 ml, and 8000 ml stainless steel beakers with the ground cork insulation between them may be replaced with a single 8000 ml glass beaker.

Test tubes, length 100 mm, diameter 25 mm with or without rim. These tubes may have an etched mark extending around the tube at a distance of 75 mm. from the bottom to show the height to which the tube is to be filled.

Stirrer, 2 to 3 mm. outside diameter, with one end bent in the form of a loop of 19 mm. outside diameter. Glass nickel chrome, stainless steel, or monel wire may be used. The upper end can be formed to accommodate hand stirring or attached to a mechanical stirrer.

Laboratory thermometer 0 - 150 °C.

Titer test thermometer ( If the titer is between 68 and 80 °C thermometers)

Reagents

1. Ethylene Glycol.

2. Dry Ice ( Solid carbon dioxide).

Procedure

Heat the fatty acids on a hot plate to 130 °C to remove traces of moisture and fill a titer test tube to a height of 57 mm from the bottom.

Caution: The sample is not held at 130 °C nor reheated to this temperature more than one. If excessive moisture is present allow the water to settle decant the fatty acids and oils and then re-filter and reheat. The acids must be dry and free of suspended matter.

For titer above 35 °C. Fill the water bath to the designated level and adjust the temperature from 15°C to 20 °C below the expected titer point. For samples with titer under 35°C use equipment as illustrated.

For titer 35 °C and below: Fill the water bath with ethylene glycol to the designated level. Insert the stainless steel screen and place dry ice just beneath the ethylene glycol level. Crush the dry ice to about 0.5 inches. cubes and add cautiously to reach the desired temperature. Maintain the temperature of the bath at 15 °C to 20 °C below the titer point of the sample.

Place the tube containing the fatty acid in the assembly as shown in the illustration. Insert the titer thermometer into the immersion mark so that it will be equidistant from the sides of the tube.

Stir with the stirring rod vertically at the rate of 100 complete up and down motions per minute. The agitation is started while the temperature is at least 10 °C above the titer point or titer value.

Stir at the directed rate until the temperature remains constant for 30 seconds or begins to rise in less than a 30-second interval. Discontinue stirring immediately remove the stirrer or raise it out of the sample and observe the increase in temperature. The titer point is the highest temperature indicated by the thermometer during this rise. Duplicate determinations are usually expected to agree within 0.2 °C.

Note:- Stirring may be performed mechanically by attaching a small motor with a suitable speed-reducing mechanism to the stirring rod.

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