قراءة كتاب Cooley's Cyclopædia of Practical Receipts and Collateral Information in the Arts, Manufactures, Professions, and Trades..., Sixth Edition, Volume II
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Cooley's Cyclopædia of Practical Receipts and Collateral Information in the Arts, Manufactures, Professions, and Trades..., Sixth Edition, Volume II
in its centre, is placed over the shoulder of the matrass, to prevent the heat from acting on the globular receiver. On the large scale, a leaden still, as before described, may be employed, and receivers of either stoneware or glass; and the addition of the sulphuric acid is made in a basin or trough of stoneware or wood. Prod. 12 oz. yield 80 to 100 gr.
4. Another method of preparing iodine has been patented by a Mr Stanford, which consists of compressing the wet weed, drying in an oven, and distilling at a high temperature. The inventor claims that double the usual amount of iodine is obtained besides other useful products.
5. Considerable quantities of iodine are now obtained from the mother-liquor of Chilian saltpetre or nitre (nitrate of soda). In 1873, a nitre refinery in Peru which separates the iodine in combination with copper, as cuprous iodide, by means of bisulphide of soda and sulphate of copper, produced 15,000 kilos of cuprous iodide, corresponding to 9000 kilos of iodine.
Other methods of obtaining it from Chilian nitre consist in treating the mother-liquors left after the salt has been crystallised out with sulphurous acid, until the separated iodine begins to redissolve. Nitrous acid has also been substituted for sulphurous. The
iodine so procured is purified by sublimation, whilst that which remains in the residual saline matter is removed by treatment with chlorine.
Prop. Iodine is usually met with under the form of semi-crystalline lumps having a semi-metallic lustre, or in micaceous, friable scales, somewhat resembling plumbago or gunpowder. By carefully conducted sublimation, or by the slow evaporation of its solution in hydriodic acid, it may be obtained in rhombic plates an inch long. It has a greyish-black colour, a hot acrid taste, and a disagreeable odour not much unlike that of chlorine. It fuses at 225° into a deep-brown liquid, volatilises slowly at ordinary temperatures, boils at 347°, forming a magnificent violet-coloured vapour, when mixed with water it rapidly rises with the steam at 212° Fahr. It dissolves in about 7000 parts of water, and freely in alcohol, ether, solutions of the iodides, liquid hydriodic acid, chloroform, petroleum, bisulphide of carbon, &c. Most of these solutions have the brown colour of liquid iodine, but some (particularly those formed by the last three solvents named above) have the beautiful violet colour of the vapour. It bleaches like chlorine, only more feebly. Iodine has an extensive range of affinity; with the metals it forms compounds termed iodides, of which several are used in medicine. Its principal compounds with oxygen are the iodic and periodic anhydrides. Sp. gr. 4·946 to 4·948. According to Debaugne, the addition of syrup of orange peel or tannin to water greatly increases its power of dissolving iodine. 2 gr. of the latter will enable 6 fl. oz. of water to take 10 gr. of iodine. A knowledge of these facts may prove useful to the pharmaceutist.
Pur. It is entirely soluble in rectified spirit, and in a solution of iodide of potassium. On applying heat to it, it first liquefies, and then (wholly) sublimes in violet-coloured vapour. The iodine of commerce is usually that of the first sublimation, and generally contains from 12% to 20% of water. Some of the foreign iodine, prepared by precipitation with chlorine, without subsequent sublimation, even contains 1-4th part of water, and has a dead leaden-grey colour, and evolves a sensible odour of chlorine. Coal, plumbago, oxide of manganese, crude antimony, and charcoal, are also frequently mixed with iodine to increase its weight. Water may be detected by the loss of weight it suffers when exposed to strong pressure between bibulous paper; or more accurately by drying it in the manner directed below,—chlorine may be detected by the odour, and the other substances mentioned above, by their insolubility in rectified spirit and in a solution of iodide of potassium. Before use as a medicine it should be dried by being placed in a shallow basin, of earthenware, in a small confined space of air, with 10 or 12 times its weight of fresh-burnt lime, till it scarcely adheres to the side of a dry bottle, or else prepared
from the commercial iodine as follows:—Place it in a deep circular porcelain capsule, and having covered it accurately with a glass matrass filled with cold water, apply a water heat to the capsule for 20 minutes, and then allow the whole to cool; should the sublimate attached to the bottom of the matrass include acicular prism of a white colour, and a pungent odour, it must be scraped off with a glass rod, and rejected; the apparatus is then to be again exposed to a gentle and steady heat until the whole of the iodine has sublimed; the sublimate is, lastly, to be collected from the bottom of the matrass, and at once enclosed in a stoppered bottle.
Tests. Free iodine may be recognised by the violet colour of its vapour, by its imparting a violet colour to bisulphide of carbon, and by its striking a blue colour with starch. The latter test is so delicate, that water containing only 1⁄450000th part of iodine acquires a perceptible blue tinge on the addition of starch. Free iodine may be eliminated from solutions of iodides by chlorine, nitric acid, concentrated sulphuric acid and peroxide of manganese, and may be made evident by adding starch-paste. This reagent serves to detect minute traces of iodine in insoluble as well as in soluble compounds of that element. The substance under examination is mixed in a retort with concentrated nitric acid, and a strip of white cotton cloth moistened with a solution of starch suspended from the stopper; in a few hours the cloth will become coloured blue if the most minute trace of iodine be present. By mixing the liquid containing the iodine with the starch and acid, and lightly pouring thereon a small quantity of aqueous chlorine, a very visible blue zone will be developed at the line of contact, even in very dilute solutions.
Iodides give a pale yellowish precipitate with nitrate of silver, scarcely soluble in ammonia, and insoluble in dilute nitric acid; a bright yellow one with acetate of lead; and a scarlet one with bichloride of mercury. This distinguishes them from the iodates which give white precipitates with the same reagents. In solutions of alkaline iodides, chloride of palladium produces a black precipitate.
Estim. The proportion of free iodine in a mixture may be estimated: by separating it by heat, and collecting and weighing the sublimate; by solution in rectified spirit, adding water, and collecting the resulting precipitate, which must then be dried and weighed; by dissolving it in a solution of iodide of potassium, and then adding a standard solution of hyposulphite of sodium, until the whole of the free iodine is taken up, and the mixture no longer strikes a blue colour with starch. 24·8 gr. of the hyposulphite are necessary to absorb 12·7 gr. of free iodine;[2]
by comparing the tint of a solution prepared by chloroform with that of a standard solution containing a known quantity of iodine, as in Crum’s process for estimating chlorine.