Some drying agents

Evidently, the types of compound compatible with this mixture are not many, but it has been used successfully for various 1,3-dioxacycloalkanes and hydrocarbons. It must not be used with halogen compounds although chloro- and bromo-alkanes can be dried safely over sodium films, provided that they are initially at least Grignard dry and free of oxygen. In the author s laboratory specimens of CHjClj and MeBr which had been over sodium films under vacuum for several years were analysed and found to contain only traces of the Wurtz-condensation products. 

Before a batch of CaHj is used, a small sample should be mixed with a few drops of water and the evolved gases smelt cautiously (or analysed by GLC). If the nose can sense phosphine or the GLC shows up acetylene, the batch should be returned to the manufacturer. Although in theory both gases would be pumped off during the reevacuation of the liquid compound to remove the hydrogen, enough might remain to interfere with catalytic reactions. 

Because of the evolution of hydrogen, it is not advisable to use CaHj for the drying of any compound, such as one containing nitro or keto groups, whose reduction would produce compounds which could interfere with the reactions to be studied. 

The possibility of an attack by the drying agent on the compound to be dried must always be considered carefully and if necessary examined by small-scale tests, as has been mentioned before. Most notable for such unwanted aggression amongst the popular drying agents is the molecular sieve. Various grades of molecular sieve have different activities and specialist publications should be consulted for details. The main reactions which must be kept in mind are that they can catalyse the dehydrochlorination of alkyl chlorides and the condensation of ketones, they can dehydrate alcohols and can form exposive compounds from nitroalkanes (see Section 4.6.3.). 

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You see that vacuum adapter stuck to the top of the condenser in fig. 7a Well, a closer look at it in fig. 7b will show that it has some drying agent sandwiched between two cotton balls and the nipple (tee heel) sealed with plastic wrap or foil. The drying agent can be either a commercial product called Drierite or calcium chloride. This attachment is placed on top of a condenser when refluxing solutions that have no water in them and must remain that way during the time they are refluxed. All this is to prevent moisture in the outside air from coming into contact with the cold surface of the of the inside walls of the condenser. This will surely happen and the condensed outside-air water will drip down into the reaction flask and ruin the experiment. This is not so much a... 

Much of what needs to be done about the techniques of removing water from glass apparatus and from solvents and reagents has been set out above in a more general context. It remains to point out a few pecularities which characterise the drying process rather than any other purification procedure and to discuss some drying agents. 

Purification, including drying 4.6.2. Some drying agents... 

It should be noted that the efficiency of some drying agents (e.g. AhO, and anhydrous CaCI>, and probably also BaO, anhydrous Mg(C10.)i, Mg(CIO,), - 3HiO, anhydrous BafCIO,) , and CaSO,) depends upon both adsorption and absorption. 

To appreciate the action of a drying agent of class (a), let us imagine some anhydrous copper sulphate in an evacuated vessel provided with a pressure gauge, and water is allowed to enter slowly the temperature is assumed constant at 25°. The results may be best expressed by means of a vapour pressure - composition diagram (Fig. 7, 20, 1). The initial system is represented by the point A the pressure will rise along AB until the monohydrate CuS04,H20 commences to form at B. 

The drying agent was filtered off on a sintered-glass funnel and rinsed with some THF. The solution was transferred into a 500-ml wide-necked flask and concentrated in a water-pump vacuum. In order to remove the last traces of THF and some water the flask was connected directly (without a column) to a condenser and a receiver, cooled at -190°. The flask was evacuated by means of a mercury pump (p < 0.1 mmHg) and heated for 1.5 h at 85°C. The greater part of the mono-... 

After drying or decomposing a sample, it should be cooled to room temperature in a desiccator to avoid the readsorption of moisture. A desiccator (Figure 2.9) is a closed container that isolates the sample from the atmosphere. A drying agent, called a desiccant, is placed in the bottom of the container. Typical desiccants include calcium chloride and silica gel. A perforated plate sits above the desiccant, providing a shelf for storing samples. Some desiccators are equipped with stopcocks that allow them to be evacuated. 

The carbon tetrachloride is dried over phosphorus pent-oxide or some other drying agent. 

The checkers purchased trifluoroacetic acid from Aldrich Chemical Company, Inc., and distilled it from phosphorous pentoxide. The submitters point out that some trifluoroacetic anhydride, whose effects have not been fully investigated, is obtained under these conditions. The submitters prefer to use trifluoroacetic acid which has been distilled through a glass packed column without the use of a drying agent. 

By the interaction of the alcohols and acids at an elevated temperature the reaction is assisted by the use of some catalytic agent, or one which absorbs the water formed, such as dry sodium acetate. The reaction is rarely complete, however, and may be rendered more nearly quantitative by using the acid anhydride in place of the acid itself. The reaction is —... 

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