CHLOROFORM
Cooley's Cyclopedia of Practical Receipts and Collateral Information · 1880 · p. 21
CHCl 3 . Syn. Terchloride of formyle , Formyl-chloride ; Chloroformyl , Tri chloromethane , Chloroformum , L. A remarkable fluid discovered by Liebig in 1830, and independently by Soubeiran in 1832, and carefully examined in 1834 by Dumas. In 1842 its action upon animals was investigated by Dr M. Glover, and in 1847 it was introduced to the medical profe ion as an anæsthetic agent by Dr Simpson of Edinburgh. It was first obtained by the action of caustic alkali upon chloral, but it is more easily prepared by distilling alcohol or wood spirit with chloride of lime. It may also be procured from wood spirit, acetone, oil of turpentine, and several e ential oils, as well as from amylic alcohol, acetic acid, tartaric acid, and phenol; when these different bodies are severally subjected to the action of chloride of lime. When chlorine is made to act on marsh gas, or when chloral is treated with an alkali, chloroform is also produced. Prep. 1. Chloride of lime (in powder), 4 lbs.; water, 12 lbs.; mix in a capacious retort or still, add of rectified spirit, 12 fl. oz., and cautiously distil as long as a dense liquid, which sinks in the water it pa es over with, is produced; separate this from the water, agitate it with a little sulphuric acid, and, lastly, rectify it from carbonate of barium. 2. Chloride of lime, 4 lbs.; water, 10 pints; rectified spirit, 1 ⁄ 2 pint; proceed as last, using a spacious retort that the mixture will only 1-3rd fill, and the heat of a sand bath. When ebullition commences remove the fire as quickly as po ible, lest the retort be broken by the suddenly increased heat, and let the solution distil into a receiver as long as there is nothing which subsides, the heat being restored if it be at all needed. Add to the distilled liquid four times as much water, and shake the whole well together; next cautiously separate the heavier part as soon as it has subsided, and to this add chloride of calcium, broken into fragments, 1 dr.; and shake occasionally during an hour; finally, let the fluid again distil from a gla retort into a gla receiver. 3. Hydrate of lime, 1 part, is suspended in cold water, 24 parts, and chlorine pa ed through the mixture until nearly the whole of the lime is di olved; hydrate of lime, q. s. just to restore the alkaline reaction of the liquid, is then added; and, afterwards, rectified spirit of wine or wood spirit, 1 part, is mixed in; the whole, after repose for 24 hours in a covered ve el, is cautiously distilled as before. 4. (B. P.) Take of chlorinated lime 10 lbs. ; rectified spirit, 30 fluid ounces; slaked lime, a sufficient quantity; water, 3 gallons; sulphuric acid, a sufficient quantity; chloride of calcium in small fragments 2 oz. ; distilled water, 10 fluid ounces. Place the water and the spirit in a capacious still, and raise the mixture to a temperature of 100° F. Add the chlorinated lime, and 5 lbs. of the slaked lime, mixing thoroughly. Connect the still with a condensing worm, encompa ed by cold water, and terminating in a narrow-necked receiver; and apply heat so as to cause distillation, taking care to withdraw the fire the moment that the proce is well established. When the distilled product measures 50 fluid ounces the receiver is to be withdrawn. Pour its contents into a gallon bottle, half filled with water; mix well by shaking, and set it at rest for a few minutes, when the mixture will separate into two strata of different densities. Let the lower stratum, which contains crude chloroform, be washed by agitating it in a bottle with 3 fluid ounces of the distilled water. Allow the chloroform to subside, withdraw the water, and repeat the washing with the rest of the distilled water, in succe ive quantities of 3 oz. at a time. Agitate the washed chloroform for five minutes in a bottle with equal volume of sulphuric acid, allow the mixture to settle, and transfer the upper stratum of liquid to a flask, containing the chloride of calcium, mixed with 1 ⁄ 2 oz. of slaked lime, which should be perfectly dry. Mix well by agitation. After the lapse of an hour connect the flask with a Liebig condenser, and distil over the pure chloroform by means of a water bath. Preserve the product in a cool place in a bottle furnished with an accurately ground stopper. The lighter liquid which floats on the crude chloroform after its agitation with water, and the washings with distilled water, should be preserved and employed in a subsequent operation. Sp. gr. 1·456. Prop., . Liquid; transparent; colourle ; odour fragrant, ethereal, and apple-like; taste ethereal, sweetish, but slightly acrid; soluble in 2000 parts of water; mixes in all proportions with alcohol and ether; di olves (readily) bromine, camphor, caoutchouc, gutta perch a, iodine, oils, resins, wax, and several other like substances; boils at 141·8° Fahr.; kindles with difficulty; burns, when strongly heated, with a greenish flame; and communicates a dull, smoky-yellow colour to the flame of alcohol. Sp. gr. 1·48 (1·497, Miller); density of vapour 4·2. The vapour has the remarkable property of rendering a person breathing it temporarily insensible to pain. Chloroform is frequently adulterated with alcohol and ether; and owing to carele manipulation, is also sometimes contaminated with other substances, as chloral, hydrochloric acid, free chlorine, aldehyde and certain chlorinated oils. These latter compounds are not only the most objectionable and prejudicial of the impurities found in chloroform, but if present in it to any appreciable extent, they render its anæsthetic administration not only inefficient, but frequently absolutely dangerous. These deleterious chlorinated oily compounds may be removed by agitation with strong sulphuric acid, or by distillation from it. Chloroform made from wood spirit is said to be more impure than that from alcohol. When pure it is free from colour, and of a pleasant odour. It is not perfectly soluble in water; and does not turn the colour of litmus red. Rubbed on the skin it quickly evaporates, scarcely leaving any odour. Dropped into water, it falls to the bottom and remains bright and limpid; but if it contain alcohol the surface of the drop becomes opaline. If the same experiment be made with diluted sulphuric acid, sp. gr. 1·44, the drop of pure chloroform will fall to the bottom; but that which contains spirit, if not shaken, will float or remain suspended in the acid solution. When contaminated with heavy hydrocarbon oils, a drop evaporated from the palm of the hand leaves behind a strong smell. Hydrochloric acid and free chlorine are detected by the ordinary tests. Mr Shuttle worth, writing to the ‘Canadian Pharmaceutical Journal,’ says:—“In regard to the restoration of chloroform which has become spoiled, I would recommend that the chloroform be well agitated with a dilute solution of hyposulphite of soda. “It should then be separated by means of a gla funnel from the supernatant liquid, and again washed; this time with simple water. After being separated the chloroform should be pa ed through filtering paper to free it from traces of moisture, when it will be found much improved and comparatively sweet, good enough in any case for external use. “There are, of course, certain other impurities of chloroform which the hyposulphite will not remove. These are of a more stable character, and as they po e a higher boiling point than chloroform, may be separated by distillation, or by treatment with sulphuric acid in the usual manner.” Uses, Action, . Chloroform is anodyne, antispasmodic, sedative, stimulant, and anæsthetic. In small doses (5 to 12 or 15 drops, in water, mixed with a little syrup or mucilage) it is employed in spasmodic disorders, and as a stimulant and diaphoretic. It is now chiefly used as an anæsthetic to produce insensibility to pain during surgical operations. The dose for inhalation is 1 fl. dr., which is repeated, in a few minutes, if no effect is produced, until 3 fl. dr. have been thus exhibited; the effects being carefully watched, and the source of the chloroform vapour removed as soon as a sufficient degree of anæsthesia is produced, or any unpleasant symptoms develop themselves. Chloroform in large doses depre es the heart’s action, and causes profound coma, and death. It is therefore dangerous in all cases complicated with diseases of the heart or brain, or any visceral affections of a congestive character. The treatment of asphyxia from chloroform is—the horizontal position, cold affusion to the head and spine, artificial respiration, and, if po ible, either the application of electricity, or the inhalation of protoxide of nitrogen or oxygen gas, largely diluted with atmospheric air. Concluding Remarks. The preparation of chloroform is not unattended with danger, and frequently miscarries in carele or inexperienced hands. This arises chiefly from the violent reaction which immediately follows the application of the heat. The common plan is attended with danger of explosion, or of the liquid in the still being forced over into the receiver, owing to the extraordinary rapidity with which the vapours are eliminated, and the ingredients, in consequence, swell up. A method which is succe fully adopted on the large scale is to employ a very broad and shallow capsule-shaped still, having a flat rim round it, with a head or capital furnished with a corresponding rim at its lower part. In use, a flat, endle band of vulcanised india rubber is placed between the two rims, which are then held air-tight together by means of small, iron clamps. The application of heat is also delayed for some time after the admixture of the spirit with the other ingredients, and the proce is interrupted as soon as the first violence of the reaction has subsided, by which time the whole product of chloroform will have pa ed over into the receiver. If the distillation is continued beyond this point, the remaining product is water. On the small scale, a very capacious, flat-bottomed retort or cucurbit should be employed. A similar condenser may be used to that noticed under ether.
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