Sometimes reagents are placed in the combustion tube, for example lead oxide (litharge), which takes up bromine and sulphur. In its simplest form the apparatus consists of a straight tube, made of glass, porcelain or iron according to the temperature required and the nature of the reacting substances, heated in an ordinary combustion furnace, the mixture entering at one end and the vapours being condensed at the other. Apparatus can also be constructed in which the unchanged vapours are continually circulated through the tube. Operating in a current of carbon dioxide facilitates the process by preventing overheating.
7. Distillation in Chemical Technology.—In laboratory practice use is made of a fairly constant type of apparatus, only trifling modifications being generally necessary to adapt the apparatus for any distillation or fractionation; in technology, on the other hand, many questions have to be considered which generally demand the adoption of special constructions for the economic distillation of different substances. The modes of distillation enumerated above all occur in manufacturing practice. Distillation in a vacuum is practised in two forms:—if the pump draws off steam as well as air it is termed a “wet” air-pump; if it only draws off air, it is a “dry” air-pump. In the glycerin industry the lyes obtained by saponifying the fats are first evaporated with “wet vacuum” and finally distilled with closed and live steam and a “dry vacuum.” Two forms of steam distillation may be distinguished:—in one the still is simply heated by a steam coil wound inside or outside the still—this is termed heating by dry steam; in the other steam is injected into the mass within the still—this is the distillation with live steam of laboratory practice. The details of the plant—the material and fittings of the still, the manner of heating, the form of the condensing plant, receivers, &c.—have to be determined for each substance to be distilled in order to work with the maximum economy.
For the distillation of liquids the retort is usually a cylindrical pot placed vertically; cast iron is generally employed, in which case the bottom is frequently incurved and thicker than the sides in order to take up the additional wear and tear. Sometimes linings of enamelled iron or other material are employed, which when worn can be replaced at a far lower cost than that of a new still. Glass stills heated by a sand bath are sometimes employed in the final distillation of sulphuric acid; platinum, and an alloy of platinum and iridium with a lining of gold rolled on (a discovery due to Heraeus), are used for the same purpose. Cast iron stills are provided with a hemispherical head or dome, generally attached to the body of the still by bolts, and of sufficient size to allow for any frothing. It is invariably provided with an opening to carry off the vapours produced. In its more complete form a still has in addition the following fittings:—The dome is provided with openings to admit (1) the axis of the stirring gear (in some stills the stirring gear rotates on a horizontal axis which traverses the side and not the head of the still), (2) the inlet and outlet tubes of a closed steam coil, (3) a tube reaching to nearly the bottom of the still to carry live steam, (4) a tube to carry a thermometer, (5) one or more manholes for charging purposes, (6) sight-holes through which the operation can be watched, and (7) a safety valve. The body of the still is provided with one or more openings at different heights to serve for the discharge of the residue in the still, and sometimes with a glass gauge to record the quantity of matter in the still. For dry distillations the retorts are generally horizontal cylinders, the bottom or lower surface being sometimes flattened. Iron and fireclay are the materials commonly employed; wrought iron is used in the manufacture of wood-spirit, fireclay for coal-gas (see Gas: Manufacture), phosphorus, zinc, &c. The vertical type, however, is employed in the manufacture of acetone and of iodine.
Several modes of heating are adopted. In some cases, especially in dry distillations, the furnace flames play directly on the retorts, in others, such as in the case of nitric acid, the whole still comes under the action of the furnace gases to prevent condensation on the upper part of the still, while in others the furnace gases do not play directly on the base or upper portion of the still but are conducted around it by a system of flues (see Coal-Tar). Steam heating, dry or live, is employed alone and also as an auxiliary to direct firing.
The condensing plant varies with the volatility of the distillate. Air cooling is adopted whenever possible. For example, in the less modern methods for manufacturing nitric acid the vapours were conducted directly into double-necked bottles (bombonnes) immersed in water. A more efficient arrangement consists of a stack of vertical pipes standing up from a main or collecting trough and connected at the top in consecutive pairs by a cross tube. By an arrangement of diaphragms in the lower trough the vapours are circulated through the system. As an auxiliary to air cooling the stack may be cooled by a slow stream of water trickling down the outside of the pipes, or, in certain cases, cold water may be injected into the condenser in the form of a spray, where it meets the ascending vapours. Horizontal air-cooling arrangements are also employed. A common type of condenser consists of a copper worm placed in a water bath; but more generally straight tubes of copper or cast iron which cross and recross a rectangular tank are employed, since this form is more readily repaired and cleansed. Wood-spirit, petroleum and coal-tar distillates are condensed in plant of the latter type. In cases where the condenser is likely to become plugged there is a pipe by means of which live steam can be injected into the condenser. The supply of water to the condenser is regulated according to the volatility of the condensate. When the vapours readily condense to a solid form the condensing plant may take the form of large chambers; such conditions prevail in the manufacture of arsenic, sulphur and lampblack: in the latter case (which, however, is not properly one of distillation) the chamber is hung with sheets on which the pigment collects. Large chambers are also used in the condensation of mercury.
Dephlegmation of the vapours arising from such mixtures as coal-tar fractions, petroleum and the “wash” of the spirit industry, is very important, and many types of apparatus are employed in order to effect a separation of the vapours. The earliest form, invented by C. B. Mansfield to facilitate the fractionation of paraffin and coal-tar distillates, consisted in having a pipe leading from the inclined delivery tube of the still to the still again, so that any vapour which condensed in the delivery tube was returned to the still. Of really effective columns Coupier’s was one of the earliest. The vapours rising from the still traverse a tall vertical column, and are then conveyed through a series of bulbs placed in a bath kept at the boiling-point of the most volatile constituent. The more volatile vapours pass over to the condensing plant, while the less volatile ones condense in the bulbs and are returned to the column at varying heights by means of connecting tubes. The French column is similar in action. The Coffey still is one of the most effective and is employed in the spirit, ammonia, coal-tar and other industries. It consists of a vertical column divided into a number of sections by horizontal plates, which are perforated so that the ascending vapours have to traverse a layer of liquid. Above this “separator” is a reflux condenser, termed the “cooler,” maintained at the correct temperature so that only the more volatile component passes to the receiver. The success of the operation chiefly depends upon the proper management of the cooler.
8. Commercial Distillation of Water.—Distilled water, i.e. water free from salts and to some extent of the dissolved gases which are always present in natural waters, is of indispensable value in many operations both of scientific and industrial chemistry. The apparatus and process for distilling ordinary water are very simple. The body of the still is made of copper, with a head and worm, or condensing apparatus, either of copper or tin. The still is usually fed continuously by the heated water from the condenser. The first portion of the distillate brings over the gases dissolved in the water, ammonia and other volatile impurities, and is consequently rejected; scarcely two-fifths of the entire quantity of water can be safely used as pure distilled water.
Apparatus for the economic production of a potable water from sea-water is of vital importance in the equipment of ships. The simple distillation of sea-water, and the production thereby of a certain proportion of chemically fresh water, is a very simple problem; but it is found that water which is merely evaporated and recondensed has a very disagreeable flat taste, and it is only after long exposure to pure atmospheric air, with continued agitation, or repeated pouring from one vessel to another, that it becomes sufficiently aerated to lose its unpleasant taste and smell and become drinkable. The water, moreover, till it is saturated with gases, readily absorbs noxious vapours to which it may be exposed. For the successful preparation of potable water from sea-water, the following conditions are essential:—1st, aeration of the distilled product so that it may be immediately available for drinking purposes; 2nd, economy of coal to obtain the maximum of water with the minimum expenditure of fuel; and 3rd, simplicity of working parts, to secure the apparatus from breaking down, and enable unskilled attendants to work it with safety. The problem is a comparatively old one, for we find that R. Fitzgerald patented a process in 1683 having for its purpose the “sweetening of sea-water.” A history of early attempts is given in S. Hales’s Philosophical Experiments, published in 1739. Among the earlier of the modern forms of apparatus which came into practical adoption are the inventions of Dr Normandy and of Chaplin of Glasgow, the apparatus of Rocher of Nantes, and that patented by Gallé and Mazeline of Havre. Normandy’s apparatus, although economical and producing water of good quality, is very complex in its structure, consisting of very numerous working parts, with elaborate arrangements of pipes, cocks and other fittings. It is consequently expensive and requires careful attention for its working. It was extensively adopted in the British navy, the Cunard line and many other important emigrant and mercantile lines. Chaplin’s apparatus, which was invented and patented later, has also since 1865 been sanctioned for use on emigrant, troop and passenger vessels. The apparatus possesses the great merit of simplicity and compactness, in consequence of which it is comparatively cheap and not liable to derangement. It was adopted by many important British and continental shipping companies, among others by the Peninsular & Oriental, the Inman, the North German Lloyd and the Hamburg American companies.
The modern distilling plant consists of two main parts termed the evaporator and condenser; in addition there must be a boiler (sometimes steam is run off the main boilers, but this practice has several disadvantages), pumps for circulating cold water in the condenser and for supplying salt water to the evaporator, and a filter through which the aerated water passes. The evaporator
