Necks

In actual practice, a weight W is obtained, which is less than the ideal value W. The reason for this becomes evident when the process of drop formation is observed closely. What actually happens is illustrated in Fig. 11-10. The small drops arise from the mechanical instability of the thin cylindrical neck that develops (see Section II-3) in any event, it is clear that only a portion of the drop that has reached the point of instability actually falls—as much as 40% of the liquid may remain attached to the tip. 

Figure C2.11.6. The classic two-particle sintering model illustrating material transport and neck growtli at tire particle contacts resulting in coarsening (left) and densification (right) during sintering. Surface diffusion (a), evaporation-condensation (b), and volume diffusion (c) contribute to coarsening, while volume diffusion (d), grain boundary diffusion (e), solution-precipitation (f), and dislocation motion (g) contribute to densification.

All the silver halides are sensitive to light, decomposing eventually to silver. In sunlight, silver chloride turns first violet and finally black. The use of these compounds in photography depends on this (see below). (All silver salts are, in fact, photosensitive—the neck of a silver nitrate bottle is black owing to a deposit of silver.)... 

The usual apparatus for heating the substance is shown in Fig. i(b), and consists of a long-necked ... 

This type of filtration is almost invariably performed with the aid of a Buchner flask and funnel, by means of which a rapid and almost complete separation can be obtained. The Buchner flask A (Fig. 4) consists of a simple thick-walled conical flask with a short side-arm for connection to a water-pump. Into the neck of the flask is fitted the Buchner funnel B which consists usually of a cylindrical porcelain funnel, the bed of which is pierced by a... 

The above units can when required be fitted into the neck of a flask by adaptors such as Fig. 22(K) and Fig. 22(L). 

The distillation heads Fig. 22(F) and Fig. 22(G) can be fitted with thermometers having a ground-glass cone just above the bulb (Fig. 22(M)). These are expensive, and it is usually more convenient to fit a thermometer pocket (Fig. 22(N)) which consists of a small well , fitting as shown into the neck of the flask. A small volume of mercury is placed in the well just to cover the bulb of a conventional thermometer, and thus provides excellent thermal contact between the thermometer and the sides of the pocket. 

Fig. 23(B) shows a modification of the reflux assembly to allow a gas to be passed through the boiling liquid cf. Fischer-Speier esterification, p. 104). The inlet-tube A fits into a three-necked adaptor shown in Fig. 22(J). The stopper B can be replaced by a dropping-funnel, etc.

Fig. 23(G) shows a three-necked round-bottomed flask A having the two side-...

Chromatographic Separation of a Mixture of o- and p-Nitroaniline. Prepare a glass tube A (Fig. 24) in which the wider portion has a diameter of 3 cm. and a length of ca. 30 cm. the narrow portion at the base has a diameter of 5-7 mm. Wash the tube thoroughly (if necessary, with chromic acid, followed by distilled water and ethanol) and then dry. Insert a small plug of cotton-wool P as shown just within the narrow neck of the tube it is essential that this plug does not project into the wider portion of the tube. Clamp the tube in a vertical position. 

To prepare pure acetylene, assemble the apparatus shown in Fig. 57. F is a wide-necked 300 ml. bolt-head flask, to which is fitted a double-surface reflux water-condenser C and the dropping-funnel D. From the top of C, a delivery-tube leads down to the pneumatic trough T, where the gas can be collected in jars in the usual way. (Alternatively, use the apparatus shown in Fig. 23(A),... 

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. 

Assemble in a fume-cupboard a 3-necked flask fitted with a stirrer, a reflux condenser, and a dropping-funnel, the apparatus... 

Picric acid if stored in bulk should, for safety, first be damped. Smaller quantities may be safely kept whilst dry, but should be stored in bottles having cork or rubber stoppers glass stoppers should never be used for potentially explosive substances, because on replacing the stopper some of the material may be ground between the neck of the flask and the stopper, and so caused to explode. 

Add 23 g. of powdered (or flake ) sodium hydroxide to a solution of 15 ml. (18 g.) of nitrobenzene in 120 ml. of methanol contained in a 250 ml. short-necked bolt-head flask. Fix a reflux water-condenser to the flask and boil the solution on a water-bath for 3 hours, shaking the product vigorously at intervals to ensure thorough mixing. Then fit a bent delivery-tube to the flask, and reverse the condenser for distillation, as in Fig. 59, p. 100, or Fig. 23(D), p. 45). Place the flask in the boiling water-bath (since methanol will not readily distil when heated on a water-bath) and distil off as much methanol as possible. Then pour the residual product with stirring into about 250 ml. of cold water wash out the flask with water, and then acidify the mixture with hydrochloric acid. The crude azoxybenzene separates as a heavy oil, which when thoroughly stirred soon solidifies, particularly if the mixture is cooled in ice-water. 

For this reduction use preferably a i litre round-bottomed flask having 3 necks (Fig. 23(G), p. 46), the two necks at the flanks being straight (to avoid the obstruction, during the addition of sodium, which a curved neck might cause). Fit the central neck with a stirrer, one of the side necks with a reflux water-condenser, and the other with a glass or rubber stopper. 

Place 5 ml. of benzaldehyde in a wide-necked stout-walled bottle of about 100 ml. capacity (a conical flask is too fragile for this purpose) and add 50 ml. of concentrated dy 0 880) ammonia solution. Cork the bottle securely, shake vigorously, and then allow to stand for 24 hours, by which time the layer of benzaldehyde at the bottom of the bottle will have been converted into a hard mass of hydrobenzamide. (If after 24 hours the crude hydrobenzamide is still syrupy, shake the mixture vigorously and allow to stand for another hour, when the conversion will be complete.) Break up the solid pellet with a strong spatula, filter at the pump, wash with water and drain thoroughly. Recrystallise from ethanol methylated spirit should not be used, as it contains sufficient water to cause partial hydrolysis back to benzaldehyde and ammonia. Hydrobenzamide is obtained as colourless crystals, m.p. 101° (and not 110° as frequently quoted) yield, 4 g. 

For this preparation, which must be performed in the fume-cupboard, assemble the apparatus shown in Fig. 67(A). C is a 150 ml. distilling-flask, to the neck of which is fitted a reflux single-surface water-condenser D, closed at the top E by a calcium chloride tube. The side-arm of C carries a cork F which fits the end E of the condenser for subsequent distillation. The side-arm of C is meanwhile plugged by a small rubber cork, or by a short length of glass rod. (Alternatively, use the ground-glass flask and condenser (Fig. 22 (a) and (c), p. 43), and... 

Place 20 g. of dry powdered benzoic acid in C, add 15 ml. (25 g., i.e., a 30% excess) of thionyl chloride and some fragments of porcelain, and then clamp the apparatus on a boiling water-bath as shown so that no liquid can collect in the side-arm of C. Heat for one hour (with occasional gentle shaking), by which time the evolution of gas will be complete. Cool the flask C, detach the condenser and fit it to the side-arm for distillation, using a 360° thermometer for the neck of C. To the lower end of the condenser fit a small conical flask G (Fig. 67(B)) by a cork carrying also a calcium chloride tube. 

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