Azeotropic Distillation Method for Moisture

V-Methylpropionamide can be dried over CaO. Water and unreacted propionic acid are removed as their xylene azeotropes. It is then distilled in a vacuum. Material used as an electrolyte solvent (specific conductance less than 10 ohm l cm ) is obtained by fractional distillation under reduced pressure, and storage over BaO or molecular sieves because it readily absorbs moisture from the atmosphere on prolonged storage. [Hoover Pure Appl Chem 37 581 1974, Recommended Methods for Purification of Solvents and Tests for Impurities, Coetzee Ed., Pergamon Press, 1982, Beilstein 4 IV 183.]... 

There are two main methods for preparation of alkyd resins. In the first one, called the fatty acid process, a free fatty acid is coesterified directly with the dibasic acid and the polyol at 200-240 °C. The reaction may be carried out without a solvent by first heating in an inert atmosphere. At the end, an inert gas may be blown into the resin from the bottom of the reaction kettle to remove water and unreacted materials. As a modification of this, a small quantity of a solvent may be used to remove water of esterification continuously by azeotropic distillation with the aid of moisture traps. 

The advantages of the coulometric method are its simplicity of operation, its increased sensitivity, and the fact that it does not require a standardized reagent, such as water saturated 1-octanol, to calculate the water content but only to assess the accuracy of the instrument. The advantage of the volumetric method is that it permits the use of a wider range of very polar solvents as well as nonpolar solvents for dissolving the sample in the titration vessel. Furthermore, the volumetric titration vessel can be heated to enhance the dissolution of slightly soluble samples. Either the volumetric or the coulometric titration instrument can be joined with an oven (evaporation) or a distillation apparatus (azeotropic distillation). In this configuration, the moisture that is volatilized from the sample can be transported to the titrator with a dry gas and the evaporated water measured either coulometrically or volumetrically. The recent... 

Moisture. The water content of lecithin products is usually less than 1.0%. As a consequence of lecithin s essentially moisture-free state, lecithin products have very low water activity and do not adversely contribute to the microbiological profile of most food systems. Most lecithin products are preserved well in storage. Higher moisture levels usually indicate a greater potential for spoilage or chemical degradation. Moisture is determined by AOCS Official Method Ja 2b-87 (77). A less accurate moisture level can also be determined by azeotropic toluene distillation (AOCS Official Method Ja 2-46) (77). One cannot determine lecithin moisture by vacuum oven methods. These methods are known to degrade lecithin products and yield false moisture levels. 

---