39. Maceration

39.    Maceration. When an infusion is made without the aid of heat it is termed maceration. This takes a much longer time than an infusion, properly so called; it rarely requires less than 7 days, sometimes several weeks. Those substances to which heat would be injurious, or which are easily soluble, are treated in this way. In many distillations this method is made use of to soften the substances before putting into the still; and to facilitate the extraction of their odorous principle.

Tinctures, when prepared by maceration, should be frequently shaken during the process, which should be conducted in glass vessels well stopped.

40. Digestion

40. Digestion is a prolonged infusion which is usually conducted at a medium temperature between that required for an infusion, properly so called, and that of a maceration. Its object is usually to impregnate alcohol with the principles of a substance which would be but slowly extracted without the aid of a certain amount of heat, such as that of the sun or of hot ashes.

Mixing together two or more liquors and allowing them to stand for some days, is also called digestion.

Maceration and digestion are usually performed in vessels of stoneware or glass, which are placed on the sand-bath, in cases where a regular and uniform heat is required.

"Whatever may be the form or nature of the vessels employed, care must be taken not to fill them full, also to cover those which are to be placed on the sand-bath with a damp piece of parchment tightly tied round the top, with many pin holes pricked in it. If this latter precaution be neglected, the increased volume produced by the heat and also the expansion of the air may burst it. Moreover, the process is never so well conducted in a vessel that is too full.

41. To obtain Tinctures by Displacement or Percolation

41. To obtain Tinctures by Displacement or Percolation. The kind or filtration commonly called the proccss of displacement, for extracting the essence from roots, herbs, seeds, barks, etc., is effected in the following manner: It is first necessary that the articles to be acted upon should be ground in a drug mill to the condition of a coarse powder; then weigh each powder by itself, and mix them together in the proportions demanded by the recipe, and moisten the mass thoroughly with alcohol, allowing it to macerate for 12 hours in a vessel well covered. Next is required a hollow instrument of cylindrical form, having one end shaped liked a funnel, so that it can be inserted in the neck of a glass bottle, and having inside, near the lower end, a partition pierced with numerous small holes, like the strainer of a French coffee-pot, which is a simple coffee percolator; in the absence of such a partition, soft cotton, or any insoluble substance, may be substituted, and being placed in the inside at the lower end of the instrument, will answer as well as the strainer. This instrument is called a percolator. Boullay's filter or percolator is usually employed. Macerate the ingredients to be acted upon, for the time named - introduce them into the percolator, and slightly press them upon the partition. Any portion of the liquid used in the maceration, not absorbed by the powder, should be poured upon the mass in the instrument, and allowed to percolate. Now gradually pour into the percolator sufficient of the alcohol, or other liquid to be filtered, to drive before it, or displace, the liquid contained in the mass; the portion introduced must in like manner be displaced by another portion; and so on, till the required quantity of filtered liquor is obtained. This extract is called a tincture. In case the liquor which first passes through should be thick and turbid, again introduce it into the instrument, being very careful not to have the powder too coarse or loosely pressed, or it will perit the liquid to pass too quickly; and on the other hand it should not be too fine and compact, or it may offer an unnecessary resistance. Should the liquor flow too rapidly, return it to the instrument, and close it beneath for a time, and thus permit the finer parts of the powder to subside, and cause a slower percolation.

The method of percolation is now preferred by all who have made sufficient trial of it to apply it correctly.

The first portion of liquid obtained by the method of displacement is always in a state of high concentration. In general it is a simple solution of the soluble ingredients of the crude drug in the fluid employed. But sometimes the solvent, if compound, is resolved into its compound parts, and the fluid which passes through it at any given time is only one of these, holding in solution only the most soluble parts of the drug.

Thus, if diluted alcohol be poured over powder of myrrh, in the cylinder of the percolator, the fluid which first drops into the receiver is a solution of an oily consistence chiefly composed of resin and volatile oil dissolved in alcohol. In like manner when the powder of gall-nuts is treated in the same way by hydrated sulphuric ether, two layers of fluid are obtained, one of which is a highly concentrated solution of tannin in the water of the ether, and the other a weak solution of the same principle in pure ether. In all cases, therefore, in which it is not otherwise directed, it is absolutely necessary to agitate the several portions of the liquid obtained by percolation together, in order to insure a product of uniform strength, or activity. To illustrate the operation of displacement, and describe an excellent percolator for making perfume tinctures, we will suppose that benzoin is under treatment. The apparatus made wholly of glass, having been arranged as shown by the engraving, and a plug of raw cotton dropped loosely at b, the benzoin in coarse powder is then poured into the tube portion, A, until it reaches the line, c. Alcohol (95 per cent.) is next added, until it rises to the line, d. As soon as the first portion sinks into the benzoin, a fresh addition must be made; and thus the succeeding relays go on displacing those which preceded them without mingling with them. Each stratum becomes more and more charged with soluble matter as it descends; and when it reaches the bottom of the mass, under the pressure of the superincumbent liquor, it runs out saturated. When, by successive additions of fresh alcohol, the benzoin under treatment has become exhausted, the liquid passes through the mass, and falls into the receiver, B, as tasteless and colorless as when first poured in. This indicates the completion of the process.

41 To obtain Tinctures by Displacement or Percolat 12

As atmospheric pressure is an important element in the operation, it will not answer to shut it off by closing the top of the displacer, without making some compensating arrangement; and, therefore, a communication between the upper and lower vessels is established by means of a latent-tube arrangement, D. In this manner the apparatus is kept close, and the evaporation of alcohol prevented, while the pressure produced is distributed throughout the apparatus, and rendered uniform. As the runnings are clear, filtration is rarely necessary. The quantity of alcohol thus consumed need not be more than sufficient to exhaust the material; and the resulting tincture must therefore be diluted to the proper strength. For perfumes, deodorized alcohol must always be used.

The method of displacement has the advantage of expedition, economy, and yielding products possessing uniformity of strength; but it requires considerable experience to adapt it to all substances. The art rests in properly packing the ingredients in the cylinder, some substances requiring considerable pressure to be used, while others, when even lightly packed, scarcely permit the fluid to pass through them. An excellent plan applicable to all substances, but especially those of a glutinous or mucilaginous nature, is to mix the powder with an equal bulk of well-washed sand, before rubbing it up with the menstruum. The coarseness of the powder must also be attended to. Substances that readily become soft and pappy when wetted by the menstruum, should not be used so fine as those that arc more woody and fibrous. The method of displacement answers well for the preparation of all tinctures that are not of a resinous nature, and for most infusions of woody and fibrous substances, as roots, woods, barks, leaves, seeds, insects, etc.. It is especially adapted for the preparation of concentrated infusions and essences, as they may thus be obtained of any required strength, without loss, or requiring concentration by heat, which is so destructive to their virtues.

When ordinary tinctures are made in large quantities, displacement is never likely to supersede maceration, on account of any practical advantages it may possess. If the prescribed directions bo duly attended to, the process of maceration is unexceptionable. The process is more simple than the other; the mode of operating more uniform; it is, in fact, always the same; it requires less of skill and dexterity in conducting it; it requires less constant attention during its progress, which, in operating on large quantities, is a consideration; and finally, the apparatus required is less complicated. When, however, only small quantities of tincture are to be made at a time, and kept in stock, the adoption of the process of displacement will often be found convenient and advantageous. It offers the means of making a tincture in two or three hours, which, by the other process, would require as many weeks. (Sec No. 4572.)