Apparatus for steam distillation

In a 12-1. flask fitted with a mechanical stirrer and a short reflux condenser are placed 1800 g. (32.2 moles) of iron filings (Note i), 3 1. (52.5 moles) of glacial acetic acid, 3 1. of water, and 450 g. (3.95 moles) of heptaldehyde (Note 2). The mixture is heated on the steam bath, with stirring, for six to seven hours (Note 3). The flask is then fitted to an apparatus for steam distillation (Org. Syn. 2, 80) and the mixture distilled in a current of steam (Note 4) until no more oil passes over (7-8 1. of distillate). The oil is then separated, and the aqueous part distilled to recover a small quantity of dissolved or suspended heptyl alcohol. 

Figure 3.64. Schematic drawing of the apparatus for steam distillation.

In the apparatus for steam distillation, the greater portion of the condensation is effected by the stream of water passing over... 

A simple apparatus for steam distillation is shown in Fig. 2.102. Flask A contains the liquid to be steam distilled it is fitted with the splash-head B which prevents the carry-over of the contents of the flask A into the receiver. To carry out a steam distillation, the solution (or mixture of the solid with a little water) is placed in the flask A, and the apparatus is completely assembled. Steam is passed into flask A, which is itself heated by means of a flame to prevent too rapid an accumulation of water. If the substance crystallises in the condenser and tends to choke it, the water should be run out of the condenser for a few minutes until the solid material has been melted and carried by the steam into the receiver the water should then be cautiously readmitted to the hot condenser. It is best to use a condenser of the double surface type if the rate at which the steam distillation is carried out is rapid if necessary two such condensers connected in series may be used since in most steam distillations best results are obtained when the process of distillation is carried out rapidly. The passage of steam is continued until no appreciable amount of water-insoluble material is... 

Alternatively, instead of setting up the apparatus for steam distillation, simply add a boiling chip to the 250-mL flask and distill 40 mL of liquid, cool the flask slightly, add 40 mL of water to it, and distill 40 mL more. Note the temperature during the distillation. This is a steam distillation in which steam is generated in situ rather than from an outside source. 

Fig. 49. Semimicro apparatus for steam distillation, using six-inch tube...

FIGURE 112. Apparatus from The Art of Distillation by John French (London, 1653 first edition, 1651) (a) Apparatus for steam distillation (b) A Balneum Marie. 

Apparatus for steam distillation with receiver and flask with reflux condenser, boiling off CO2... 

Apparatus A 125-mL separatory funnel, a 125-mL round-bottom flask, and apparatus for steam distillation using an internal steam source, simple distillation, and flameless heating. 

Isolation While the reaotion mixture is cooling, prepare an apparatus for steam distillation with internal steam generation. Add about 35-40 ml of water to the reaction flask. Heat the flask and steam-distill the product until about 30-35 ml of... 

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