Distilling flask

42 Heating The two most common heat sources for distillation flasks are oil baths and heating mantles, both described in Sec. 1.7.1. The heat source should allow fine adjustment of the heat input rate and ideally should apply the heat uniformly to avoid local superheating with resultant decomposition (more of a problem with heating mantles than with oil baths). 

3 Distilling Flasks Distilling flasks are available in many sizes and shapes and are frequently designed for a specific type of column. If a choice 

---

Experimental Determination of Boiling-point. Unless only minute quantities of the liquid are available cj. p. 60), the boiling-point is usually determined by simple distillation. For this purpose, the apparatus shown in Fig. 2 is assembled. A distillation flask A of suitable size is fitted to a water-condenser B, the water supply of which is arranged as show-n. An adaptor C is sometimes fitted in turn to the condenser, so that the distillate... 

The thermometer should be so arranged that the top of the bulb is just level with the centre of the side-arm of the distilling-flask. 

Distillation. If the impurities in a liquid are non-volatile, the liquid may be purified by direct distillation, the impurities remaining in the distilling-flask. This process is therefore essentially the same as a simple distillation for boiling-point determination, and has been already described on pp. 7-9. 

If, however, the impurities are themselves volatile liquids, then the separation of these impurities from the main bulk of the required substance is achieved by fractional distillation. If an ordinary distilling-flask, such as that shown in Fig. 2, p. 8, is used for this purpose, however, only a very partial separation of the liquid components of the crude mixture is usually obtained, unless there is a considerable difference in boiling-point between the impurities and the main component. T0 obtain a much sharper and more complete separation, a fractionating column is employed. 

Concentrate each of the two solutions (or eluates) to about 20 ml, by distilling off the greater part of the benzene, the distilling-flask being immersed in the boiling water-bath. Then pour the concentrated solution into an evaporating-basin, and evaporate the remaining benzene (preferably in a fume-cupboard) in the absence of free flames, i.e., on an electrically heated water-bath, or on a steam-bath directly connected to a steam-pipe. Wash the dry residue from the first eluate with petrol and then dry it in a desiccator pure o-nitroaniline, m.p. 72°, is obtained. Wash the second residue similarly with a small quantity of benzene and dry pure />--nitroaniline, m.p. 148" , is obtained. Record the yield and m.p. of each component. 

Now filter the ether through a fluted filter-paper directly into a 100 ml. distilling-flask, and then equip the latter with a 100° thermometer and a double-surface condenser to the end of the latter attach a receiver with a rubber delivery-tube precisely as before. Place the flask cautiously in a water-bath, the contents of which have previously been heated to about 60° at some distance from the apparatus arrange the depth of the flask in the water-bath so that the ether distils slowly over. Collect the fraction boiling between 34-39°. Yield, 25 g. (35 ml.). Not more than a verv small residue of etlianol should remain in the flask. 

Hydrolysis of Acetoxime. Place about i g. of the recrystallised oxime in a small distilling-flask (50 ml.), add 10 ml. of dilute HjSO, and heat gently until about half the solution has distilled over. Test [a] the aqueous distillate for acetone by the iodoform reaction (p.346), b) the residual solution in the distilling-flask for hydroxylamine by... 

After about 20 minutes, when the liquid should be dry, filter it through a small fluted filter-paper into a 100 ml. distilling-flask attached to a water-condenser. Add some fragments of unglazed porcelain to the ethyl acetate, fit a 100° thermometer to the flask, and place the latter on a cold water-bath, which is then brought to the boil. Some ether is always formed as a by-product with the ethyl acetate, and by these means is carefully distilled off as a... 

Now decant the dried liquid into a small distilling flask of about 10 ml, capacity (Fig. 36, p. 63). Distil the liquid and collect the fraction b.p. 74-79°. Yield, 3 g. 

A considerable amount of the formic acid, however, still remains behind in the distilling-flask as the unhydrolysed monoformate. Therefore, if time allows, dilute the residue in the flask with about an equal volume of water, and then steam-distil, the monoformate ester being thus completely hydrolysed and the formic acid then driven over in the steam. Collect about 400 ml. of distillate. Add this distillate to that obtained by direct heating of the reaction mixture and then treat with lead carbonate as described above. Total yield of lead formate is now about 40 g. 

The crude acetonitrile contains as impurity chiefly acetic acid, arising from the action of phosphoric acid on the acetamide. Therefore add to the nitrile about half its volume of water, and then add powdered dry potassium carbonate until the well-shaken mixture is saturated. The potassium carbonate neutralises any acetic acid present, and at the same time salts out the otherwise water-soluble nitrile as a separate upper layer. Allow to stand for 20 minutes with further occasional shaking. Now decant the mixed liquids into a separating-funnel, run off the lower carbonate layer as completely as possible, and then pour off the acetonitrile into a 25 ml, distilling-flask into which about 3-4 g. of phosphorus pentoxide have been placed immediately before. Fit a thermometer and water-condenser to the flask and distil the acetonitrile slowly, collecting the fraction of b.p. 79-82°. Yield 9 5 g. (12 ml.). 

Meanwhile assemble the apparatus shown in Fig. 62, or that in Fig. 23(D), p. 45, having a distilling-flask of at least 500 ml. capacity in either case. If an ordinary condenser C (Fig. 62) is employed, fit the lower end of the condenser by means of a short piece of rubber tubing to a small inverted funnel. Arrange the latter so that its lip is just below the surface of 25 ml. of concentrated hydrochloric acid diluted with 75 ml. of water contained in a 250 ml. beaker B the hydro-. chloric acid is thereby prevented from being sucked back into the... 

Add 15 g, of chloroacetic acid to 300 ml. of aqueous ammonia solution d, o-88o) contained in a 750 ml. conical flask. (The manipulation of the concentrated ammonia should preferably be carried out in a fume-cupboard, and great care taken to avoid ammonia fumes.) Cork the flask loosely and set aside overnight at room temperature. Now concentrate the solution to about 30 ml. by distillation under reduced pressure. For this purpose, place the solution in a suitable distilling-flask with some fragments of unglazed porcelain, fit a capillary tube to the neck of the flask, and connect the flask through a water-condenser and receiver to a water-pump then heat the flask carefully on a water-bath. Make the concentrated solution up to 40 ml. by the addition of water, filter, and then add 250 ml. of methanol. Cool the solution in ice-water, stir well, and set aside for ca. I hour, when the precipitation of the glycine will be complete. 

Add cautiously 15 ml. of concentrated sulphuric acid to 50 ml. of water in a 100 ml. distilling-flask, and then add 10 g. of pinacol hydrate. Distil the solution slowly. When about 40 ml. of distillate (consisting of pinacolone and water) have been collected, and no more pinacolone comes over, extract the distillate with ether. Dry the extract over sodium sulphate. Distil the dry filtered extract carefully, with the normal precautions for ether distillation (p. 164). When the ether has been removed, continue the distillation slowly, rejecting any fraction coming over below 100 . Collect the pinacolone, b.p. 106 , as a colourless liquid having a peppermint odour. Yield, 4 5-5 o g. A small quantity of higher-boiling material remains in the flask. 

Carefully refractionate the liquid of b.p. 150-160°, either by direct distillation from a small distilling-flask or (preferably) by using a short fractionating column, of the type shown in Fig. ii(b), p. 26. Almost pure bromobenzene is thus obtained, of... 

Filter the dried ethereal solution, and then distil off the ether from a small flask, using precisely similar apparatus and the same method as those described in the preparation of aniline (Fig. 64, p. 163 see also Fig. 23(E), p. 45) and observing the same precautions. When the ether has been removed, fit the distilling-flask to a short air-condenser, and distil the benzonitrile, collecting the fraction boiling between 187" and 191°. Yield, 16-5 g. (16 ml.). 

In order to save the cost of the distilling-flask (which after the above treatment is useless for further work), the mixture may be distilled from a small retort made by blowing a suitable bulb on the end of a rather thick-walled tube of about 8-10 mm. internal diameter the tube is then bent through almost 90° a few cm. above the bulb, cut to a suitable length, and the Open end fitted into the boiling ube as before. 

Place 80 g, of hydroxylamine sulphate (or 68-5 g. of the hydrochloride), 25 g. of hydrated sodium acetate, and 100 ml. of water in a 500 ml. flask fitted with a stirrer and a reflux water-condenser, and heat the stirred solution to 55-60°. Run in 35 g (42 nil,) of -hexyl methyl ketone, and continue the heating and vigorous stirring for ij hours. (The mixture can conveniently be set aside overnight after this stage.) Extract the oily oxime from the cold mixture twice with ether. Wash the united ethereal extract once with a small quantity of water, and dry it with sodium sulphate. Then distil off the ether from the filtered extract, preferably using a distillation flask of type shown in Fig. 41 (p. 65) and of ca, 50 ml, capacity, the extract being run in as fast as the ether distils, and then fractionally distil the oxime at water-pump pressure. Collect the liquid ketoxime, b.p. 110-111713 mm. Yield, 30-32 g. 

---