Chapter XXXVIII: Section III: The ANALYSIS of MINERAL SUBSTANCES (2)
All the vessels above-mentioned are fit only for distilling such light volatile matters as can be easily raised and brought over; such as phlegm, essential oils, fragrant waters, acid oily spirits, volatile alkalis, _&c._ But when the point is to procure by distillation principles that are much less volatile, and incapable of rising high, such as the thick fetid oils, the vitriolic, the nitrous, and the marine acids, _&c._ we are under a necessity of having recourse to other vessels, and another manner of distilling.
It is easy to imagine, that such a vessel must be much lower than the alembic. It is indeed no more than a hollow globe, whose upper part degenerates into a neck or tube, that is bent into a horizontal position; for which reason this instrument is called a _Retort_: it is always of one single piece.
The matter to be distilled is introduced into the body of the retort by means of a ladle with a long tubular shank. Then it is set in a furnace built purposely for this use, and so that the neck of the retort coming out of the furnace may, like the nose of the alembic, stand in a sloping position, to facilitate the egress of the liquors, which by its means are conveyed to a receiver, into which it is introduced, and with which it is luted. This way of distilling, in which the vapours seem rather to be driven out of the vessel horizontally and laterally, than raised up and sublimed, is for that reason called Distillation _per Latus_.
Retorts are, of all the instruments of distillation, those that must sustain the greatest heat, and resist the strongest solvents; and therefore they must not be made of metal. Some, however, which are made of iron may do well enough on certain occasions: the rest are either of glass or earth. Those of glass, for the reasons above given, are preferable to the other sort, in all cases where they are not to be exposed to such a force of fire as may melt them. The best glass, that which stands both heat and solvents best, is that in which there are fewest alkaline salts. Of this sort is the green German glass: the beautiful white crystal glass is far from being equally serviceable.
Retorts, as well as alembics, may be of different forms. For example, some matters are apt to swell, and rise over the neck of the retort in substance, without suffering any decomposition; when such matters are to be distilled in a retort, it is proper that the body of the vessel, instead of being globular, be drawn out into the form of a pear, so as nearly to resemble that of a cucurbit. In a retort of this kind, the distance between the bottom and the neck being much greater than in those whose bodies are spherical, the matters contained have much more room for expansion; so that the inconvenience here mentioned is thereby prevented. Retorts of this form are called English retorts. As they hold the middle place between alembics and common retorts, they may be used to distil such matters as have a mean degree of volatility between the greatest and the least.
It is moreover proper to have, in a laboratory, sundry retorts with necks of different diameters. Wide necks will be found the fittest for conveying thick matters, and such as readily become fixed; for instance, some very thick fetid oils, butter of antimony, _&c._; for as these matters acquire a consistence as soon as they are out of the reach of a certain degree of heat, they would soon choak a narrow neck, and by stopping the vapours which rise at the same time from the retort, might occasion the bursting of the vessels.
Some retorts are also made with an opening on their upper side, like that of tubulated glass alembics, which is to be closed in the same manner with a glass stopple. These retorts are also called Tubulated retorts, and ought always to be used whenever it is necessary to introduce fresh matter into the retort during the operation; seeing it may be done by means of this invention, without unluting and reluting the vessels; which ought always to be avoided as much as possible.
One of the things that most perplexes the Chymists, is the prodigious elasticity of many different vapours, which are frequently discharged with impetuosity during the distillation, and are even capable of bursting the vessels with explosion, and with danger to the artist. On such occasions it is absolutely necessary to give these vapours vent, as we shall direct in its proper place: but as that can never be done without losing a great many of them; as some of them in particular are so elastic that scarce any at all would remain in the vessel; for instance, those of the spirit of nitre, and especially those of the smoking spirit of salt; the practice is to make use of very large receivers, of about eighteen or twenty inches diameter, that the vapours may have sufficient room to circulate in, and by applying to the wide surface presented them by the extensive inside of such a large vessel, may be condensed into drops. These huge receivers are commonly in the form of hollow globes, and are called Ballons.
To give these vapours still more room, ballons have been contrived with two open gullets in each, diametrically opposite to one another; whereof one admits the neck of the retort, and the other is received by one of the gullets of a second ballon of the same form, which is joined in like manner to a third, and so on. By this artifice the space may be enlarged at pleasure. These ballons with two necks are called Adopters.
Operations on bodies that are absolutely fixed, as metals, stones, sand, _&c._ require only such vessels as are capable of containing those bodies, and resisting the force of fire. These vessels are little hollow pots, of different dimensions, which are called Crucibles. Crucibles can hardly be made of any thing but earth; they ought to have a cover of the same material fitted to shut them close. The best earth we know is that whereof those pots are made in which butter is brought from Bretagne: these pots themselves are exceeding good crucibles; and they are almost the only ones that are capable of holding glass of lead in fusion, without being penetrated by it.
For the roasting of ores, that is, freeing them, by the help of fire, from their sulphureous and arsenical parts, little cups of the same material with crucibles are used; but they are made flat, shallow, and wider, above than below, that these volatile matters may the more freely exhale. These vessels are called Tests, or Scorifiers: they are scarce ever used but in the Docimastic art, that is, in making small Assays of ores.
CHAP. XIX.
_The_ THEORY _of_ CONSTRUCTING _the_ FURNACES _most commonly used in_ CHYMISTRY.
Skill in conducting and applying fire properly, and determining its different degrees, is of very great consequence to the success of Chymical operations.
As it is exceeding difficult to govern and moderate the action of fire, when the vessels in which any operation is performed are immediately exposed to it, Chymists have contrived to convey heat to their vessels, in nice operations, through different mediums, which they place occasionally between those vessels and the fire.
Those intermediate substances in which they plunge their vessels are called Baths. They are either fluid or solid: the fluid baths are water or its vapours. When the distilling vessel is set in water, the bath is called _Balneum Mariæ_, or the _Water Bath_; and the greatest degree of heat of which it is susceptible is that of boiling water. When the vessel is exposed only to the vapours which exhale from water, this forms the _Vapour Bath_; the heat of which is nearly the same with that of the _Balneum Mariæ_. These baths are useful for distilling essential oils, ardent spirits, sweet-scented waters; in a word, all such substances as cannot bear a greater heat, without prejudice either to their odour, or to some of their other qualities.
Baths may also be made of any other fluids, such as oils, mercury, _&c._ which are capable of receiving and communicating much more heat: but they are very seldom used. When a more considerable degree of heat is required, a bath is prepared of any solid matter reduced to a fine powder, such as sand, ashes, filings of iron, _&c._ The heat of these baths may be pushed so far as to make the bottom of the vessel become faintly red. By plunging a thermometer into the bath, by the side of the vessel, it is easy to observe the precise degree of heat applied to the substance on which you are working. It is necessary that the thermometers employed on this occasion be constructed on good principles, and so contrived as to be easily compared with those of the most celebrated natural philosophers. Those of the illustrious Réaumur are most used and best known, so that it would not be amiss to give them the preference. When a greater heat is required than any of those baths can give, the vessels must be set immediately on live coals, or in a flaming fire: this is called working with a naked fire; and, in this case it is much more difficult than in the other to determine the degrees of heat.
There are several ways of applying a naked fire. When the heat or flame is reflected upon the upper part of a vessel which is exposed to the fire, this is called a Reverberated heat. A Melting heat is that which is strong enough to fuse most bodies. A Forging heat is that of a fire which is forcibly excited by the constant blast of a pair of bellows, or more.
There is also another sort of fire which serves very commodiously for many operations, because it does not require to be fed or frequently mended: this is afforded by a lamp with one or more wicks, and may be called a Lamp-heat. It is scarce ever employed but to heat baths, in operations which require a gentle and long continued warmth: if it hath any fault, it is that of growing gradually hotter.
All the different ways of applying fire require Furnaces of different constructions: we shall therefore describe such as are of principal and most necessary use.
Furnaces must be divided into different parts or stories, each of which has its particular use and name.
The lower part of the furnace, designed for receiving the ashes and giving passage to the air, is called the Ash-hole. The ash-hole is terminated above by a grate, the use of which is to support the coals and wood, which are to be burnt thereon: this part is called the Fire-place. The fire-place is in like manner terminated above by several iron bars, which lie quite across it from right to left, in lines parallel to each other: the use of these bars is to sustain the vessels in which the operations are to be performed. The space above these bars to the top of the furnace is the upper story, and may be called the Laboratory of the furnace. Lastly, some furnaces are quite covered above by means of a kind of vaulted roof called the Dome.
Furnaces have moreover several apertures: one of these is at the ash-hole, which gives passage to the air, and through which the ashes that fall through the grate are raked out; this aperture is called the ash-hole Door: another is at the fire-place, through which the fire is supplied with fuel, as occasion requires; this is called the mouth or door of the Fire-place, or the Stoke-hole: there is a third in the upper story, through which the neck of the vessel passes; and a fourth in the dome for carrying off the fuliginosities of combustible matters, which is called the Chimney.
To conclude, there are several other openings in the several parts of the furnace, the use whereof is to admit the air into those places, and also, as they can be easily shut, to incite or slacken the activity of the fire, and so to regulate it; which has procured them the title of Registers. All the other openings of the furnace should be made to shut very close, the better to assist in governing the fire; by which means they likewise do the office of registers.
In order to our forming a just and general idea of the construction of furnaces, and of the disposition of the several apertures in them, with a view to increase or diminish the activity of the fire, it will be proper to lay down, as our ground-work, certain principles of natural philosophy, the truth of which is demonstrated by experience.
And first, every body knows that combustible matters will not burn or consume unless they have a free communication with the air; insomuch that if they be deprived thereof, even when burning most rapidly, they will be extinguished at once: that consequently combustion is greatly promoted by the frequent accession of fresh air, and that a stream of air, directed so as to pass with impetuosity through burning fuel, excites the fire to the greatest possible activity.
Secondly, it is certain that the air which touches, or comes near ignited bodies is heated, rarefied, and rendered lighter than the air about it, that is, farther distant from the center of heat; and consequently that this air, so heated and become lighter, is necessarily determined thereby to ascend and mount aloft, in order to make room for that which is less heated and not so light, which by its weight and elasticity tends to occupy the place quitted by the other. Another consequence hereof is, that if fire be kindled in a place enclosed every where but above and below, a current of air will be formed in that place, running in a direction from the bottom to the top; so that if any light bodies be applied to the opening below, they will be carried up towards the fire; but, on the contrary, if they be held at the opening above, they will be impelled by a force which will drive them up, and carry them away from the fire.
Thirdly and lastly, it is a truth demonstrated in hydraulics, that the velocity of a given quantity of any fluid, determined to flow in any direction whatever, is so much the greater the narrower the channel is to which that fluid is confined; and consequently that the velocity of a fluid will be increased by making it run from a wider through a narrower passage.
These principles being established, it is easy to apply them to the construction of furnaces. First, if a fire be kindled in the fire-place of a furnace, which is open on all sides, it burns nearly as if it were in the open air. It has with the surrounding air a free communication; so that fresh air is continually admitted to facilitate the entire combustion of the inflammable matters employed as fuel. But there being nothing to determine that air to pass with rapidity through the fire in this case, it does not at all augment the activity thereof, but suffers it to waste away quietly.
Secondly, if the ash-hole or dome of a furnace, in which a fire is burning, be shut quite close, then there is no longer any free communication between the air and the fire: if the ash-hole be shut, the air is debarred from having free access to the fire; if the dome be stopt, the egress of the air rarefied by the fire is prevented; and consequently the fire must in either case burn very faintly and slowly, gradually die away, and at last go quite out.
Thirdly, if all the openings of the furnace be wholly closed, it is evident that the fire will be very quickly extinguished.
Fourthly, if only the lateral openings of the fire-place be shut, leaving the ash-hole and upper part of the furnace open; it is plain that the air entering by the ash-hole will necessarily be determined to go out at top, and that consequently a current of air will be formed, which will pass through the fire, and make it burn briskly and vigorously.
Fifthly, if both the ash-hole and the upper story of the furnace be of some length, and form canals either cylindric or prismatic, then the air being kept in the same direction through a longer space, the course of its stream will be both stronger and better determined, and consequently the fire will be more animated by it.
Sixthly and lastly, if the ash-hole and the upper part of the furnace, instead of being cylindric or prismatic canals, have the form of truncated cones or pyramids, standing on their bases, and so ordered that the upper opening of the ash-hole, adjoining to the fire-place, may be wider than the base of the superiour cone or pyramid, then the stream of air, being forced to pass incessantly from a larger channel through a smaller, must be considerably accelerated, and procure to the fire the greatest activity which it can receive from the make of a furnace.
The materials fittest for building furnaces are, 1. Bricks, joined together with potters clay mixed with sand and moistened with water. 2. Potters clay mingled with potsherds, moistened with water, and baked in a violent fire. 3. Iron; of which all furnaces may be made, with this precaution, that the inside be provided with a great many prominent points, as fastenings for a coat of earth, with which the internal parts of the furnace must necessarily be covered to defend it from the action of the fire.
The reverberating furnace is one of those that are most employed in Chymistry: it is proper for distillations by the retort, and should be constructed in the following manner.
First, the use of the ash-hole being, as was said, to give passage to the air and to receive the ashes, no bad consequence can attend its being made pretty high: it may have from twelve to twenty or twenty-four inches in heighth. Its aperture should be wide enough to admit billets of wood, when a great fire is to be made.
Secondly, the ash-hole must be terminated at its upper part by an iron grate, the bars of which should be very substantial, that they may resist the action of the fire: this grate is the bottom of the fire-place, and destined to support the coals. In the lateral part of the fire-place, and nearly about the same heighth with the grate, there should be a hole of such a size that it may easily admit charcoal, as well as little tongs and shovels for managing the fire. This aperture or mouth of the fire-place should be perpendicularly over the mouth of the ash-hole.
Thirdly, from six to eight or ten inches high above the grate over the ash-hole, little apertures must be made in the walls of the furnace, of eight or ten lines in diameter, an inch from one another, and those in one side must be diametrically opposite to those in the other. The use of these holes is to receive bars of iron for the retort to rest on; which should be, as I said, at different heights, in order to accommodate retorts of different sizes. At the upper extremity of this part of the furnace, which reaches from the iron bars to the top, the heighth whereof should be somewhat less than the width of the furnace, must be cut a semi-circular aperture for the neck of the retort to come through. This hole must by no means be over the doors of the fire-place and ash-hole; for then, as it gives passage to the neck of the retort, it must of course be opposite to the receiver, and in that case the receiver itself would stand over against those two apertures; which would be attended with this double inconvenience, that the receiver would not only grow very hot, but greatly embarrass the operator, whose free access to the fire-place and ash-hole would be thereby obstructed. It is proper therefore that the semi-circular cut we are speaking of be so placed that when the greatest ballons are luted to the retort they may leave an open passage to the fire-place and ash-hole.
Fourthly, in order to cover in the laboratory of the reverberating furnace, there must be a roof made for it in the form of a cupola, or concave hemisphere, having the same diameter as the furnace. This dome should have a semi-circular cut in its rim, answering to that above-directed to be made in the upper extremity of the furnace, so that, when adjusted to each other, the two together may form a circular hole for the neck of the retort to pass through. At the top of this dome there must also be a circular hole of three or four inches diameter, carrying a short tapering funnel of the same diameter, and three inches high, which will serve for a chimney to carry off all fuliginosities, and accelerate the current of the air. This passage may be shut at pleasure with a flat cover. Moreover, as it is necessary that the dome should be taken off and put on with ease, it should have two ears or handles for that purpose: a portative or moveable furnace should also have a pair of handles, fixed opposite to each other, between the ash-hole and the fire-place.
Sixthly and lastly, a conical canal must be provided of about three feet long, and sufficiently wide at its lower end to admit the funnel of the aperture at the top of the dome. This conical tube is to be applied to the dome when the fire is required to be extremely active: it tapers gradually from its base upwards, and breaks off as if truncated at top, where it should be about two inches wide.
Besides the apertures already mentioned as necessary to a reverberating furnace, there must also be many other smaller holes made in its ash-hole, fire-place, laboratory, and dome, which must all be so contrived as to be easily opened and shut with stopples of earth: these holes are the registers of the furnace, and serve to regulate the activity of the fire, according to the principles before laid down.
When the action of the fire is required to be exactly uniform and very brisk, it is necessary to stop carefully with moist earth all the little chinks in the juncture of the dome with the furnace, between the neck of the retort and the circular hole through which it passes, and which it never fills exactly, and, lastly, the holes which receive the iron bars that sustain the retort.
It is proper to have, in a laboratory, several reverberating furnaces of different magnitudes; because, they must be proportioned to the size of the retorts employed. The retort ought to fill the furnace, so as to leave only the distance of an inch between it and the inside of the furnace.
Yet when the retort is to be exposed to a most violent fire, and especially when it is required that the heat shall act with equal force on all parts of the furnace, and as strongly on its vault as on its bottom, a greater distance must be left between the retort and the inside of the furnace; for then the furnace may be filled with coals, even to the upper part of the dome. If moreover some pieces of wood be put into the ash-hole, the conical canal fitted on to the funnel of the dome, and all the apertures of the furnace exactly closed, except the ash-hole and the chimney, the greatest heat will then be excited that this furnace can produce.
The furnace now described may also be employed in many other chymical operations. If the dome be laid aside, an alembic may very well be placed therein: but then the space, which will be left between the body of the alembic and the top of the upper part of the furnace, must be carefully filled up with Windsor-loam moistened; for without that precaution the heat will soon reach the very head, which ought to be kept as cool as possible, in order to promote the condensation of the vapours. On this occasion therefore it will be proper to leave no holes open in the fire-place, but the lateral ones; of which also those over-against the receiver must be stopped.
A pot, or broad-brimmed earthen pan, may be placed over this furnace, and being so fitted to it as to close the upper part thereof accurately, and filled with sand, may serve for a sand-heat to distil with.
The bars designed to support distilling vessels being taken out, a crucible may stand therein, and many operations be performed that do not require the utmost violence of fire. In a word, this furnace is one of the most commodious that can be, and more extensively useful than any other.
The Melting furnace is designed for applying the greatest force of heat to the most fixed bodies, such as metals and earths. It is never employed in distilling: it is of no use but for calcination and fusion; and consequently need not admit any vessels but crucibles.
The ash-hole of this furnace differs from that of the reverberating furnace only in this, that it must be higher, in order to raise the fire-place to a level with the artist's hand; because in that all the operations of this furnace are performed. The ash-hole therefore must be about three feet high: and this heighth procures it moreover the advantage of a good draught of air. For the same reason, and in consequence of the principles we laid down, it should be so built that its width lessening insensibly from the bottom to the top, it may be narrower where it opens into the fire-place than any where below.
The ash-hole is terminated at its upper end, like that of the reverberating furnace, by a grate, which serves for the bottom of the fire-place, and ought to be very substantial, that it may resist the violence of the fire. The inside of this furnace is commonly an elliptic curve; because it is demonstrated by mathematicians that surfaces having that curvature reflect the rays of the sun, or of fire, in such a manner, that meeting in a point, or a line, they produce there a violent heat. But, to answer this purpose, those surfaces must be finely polished; an advantage hardly procurable to the internal surface of this furnace, which can be made of nothing but earth: besides, if it were possible to give it a polish, the violent action of the fire that must be employed in this furnace would presently destroy it. Yet the elliptical figure must not be entirely disregarded: for, if care be taken to keep the internal surface of the furnace as smooth as possible, it will certainly reflect the heat pretty strongly, and collect it about the center.
The fire-place of this furnace ought to have but four apertures.
First, that of the lower grate, which communicates with the ash-hole.
Secondly, a door in its fore-side, through which may be introduced coals, crucibles, and tongs for managing them: this aperture should be made to shut exactly with a plate of iron, having its inside coated with earth, and turning on two hinges fixed to the furnace.
Thirdly, over this door a hole slanting downwards, towards the place where the crucible is to stand. The use of this hole is to give the operator an opportunity of examining the condition of the matters contained in his crucible without opening the door of the fire-place: this hole should be made to open and shut easily, by means of a stopple of earth.
Fourthly, a circular aperture of about three inches wide in the upper part or vault of the furnace, which should gradually lessen and terminate, like that of the dome of the reverberating furnace, in a short conical funnel of about three inches long, and fitted to enter the conical pipe before described, which is applied when the activity of the fire is to be increased.
When this furnace is to be used, and a crucible to be placed in it, care must be taken to set on the grate a cake of baked earth, somewhat broader than the foot of the crucible. The use of this stand is to support the crucible, and raise it above the grate, for which purpose it should be two inches thick. Were it not for this precaution the bottom of the crucible, which would stand immediately on the grate, could never be thoroughly heated, because it would be always exposed to the stream of cold air which enters by the ash-hole. Care should also be taken to heat this earthen bottom red-hot before it be placed in the furnace, in order to free it from any humidity, which might otherwise happen to be driven against the crucible during the operation, and occasion its breaking.
We omitted to take notice, in speaking of the ash-hole, that, besides its door, it should have about the middle of its heighth a small hole, capable of receiving the nosel of a good perpetual bellows, which is to be introduced into it and worked, after the door is exactly shut, when it is thought proper to excite the activity of the fire to the utmost violence. The Forge is only a mass of bricks of about three feet high, along whose upper surface is directed the nose or pipe of a pair of large perpetual bellows, so placed that the operator may easily blow the fire with one hand. The coals are laid on the hearth of the forge near the nose of the bellows; they are confined, if necessary, to prevent their being carried away by the wind of the bellows, within a space inclosed by bricks; and then by pulling the bellows the fire is continually kept up in its greatest activity. The forge is of use when there is occasion to apply a great degree of heat suddenly to any substance, or when it is necessary that the operator be at liberty to handle frequently the matters which he proposes to fuse or calcine.
The Cupelling furnace is that in which gold and silver are purified, by the means of lead, from all alloy of other metallic substances. This furnace must give a heat strong enough to vitrify lead, and therewith all the alloy which the perfect metals may contain. This furnace is to be built in the following manner.
First, of thick iron plates, or of some such composition of earth as we recommended for the construction of furnaces, must be formed a hollow quadrangular prism, whose sides may be about a foot broad, and from ten to eleven inches high; and extending from thence upwards may converge towards the top, so as to form a pyramid truncated at the heighth of seven or eight inches, and terminated by an aperture of the width of seven or eight inches every way. The lower part of the prism is terminated, and closed, by a plate of the same materials of which the furnace is constructed.
Secondly, in the fore-side or front of this prism there is an opening of three or four inches in heighth, by five or six inches in breadth: this opening, which should be very near the bottom, is the door of the ash-hole. Immediately over this opening is placed an iron grate, the bars of which are quadrangular prisms of half an inch square, laid parallel to each other, and about eight or nine inches asunder, and so disposed that two of their angles are laterally opposite, the two others looking one directly upwards and the other downwards. As in this situation the bars of the grate present to the fire-place very oblique surfaces, the ashes and very small coals do not accumulate between them, or hinder the free entrance of the air from the ash-hole. This grate terminates the ash-hole at its upper part, and serves for the bottom of the fire-place.
Thirdly, three inches, or three and a half, above the grate, there is in the fore-side of the furnace another opening, terminated by an arch for its upper part, which consequently has the figure of a semi-circle: it ought to be four inches wide at bottom, and three inches and an half high at its middle. This opening is the door of the fire-place; yet it is not intended for the same uses as the door of the fire-place in other furnaces: the purpose for which it is actually destined shall be explained when we come to shew how the furnace is to be used. An inch above the door of the fire-place, still in the fore-side of the furnace, are two holes of about an inch diameter, and at the distance of three inches and a half from each other, to which answer two other holes of the same size, made in the hinder part, directly opposite to these. There is, moreover, a fifth hole of the same width about an inch above the door of the fire-place. The design of all these holes shall be explained when we describe the manner in which these furnaces are to be used.
Fourthly, the fore-part of the furnace is bound by three iron braces, one of which is fixed just below the door of the ash-hole; the second occupies the whole space between the ash-hole door and the door of the fire-place, and has two holes in it, answering to those which we directed to be made in the furnace itself about this place; and the third is placed immediately over the door of the fire-place. These braces must extend from one corner of the front of the furnace to the other, and be fastened thereto with iron pins, in such a manner that their sides next to the doors may not lie quite close to the body of the furnace, but form a kind of grooves for the iron plates to slide in, that are designed to shut the two doors of the furnace when it is necessary. Each of these iron plates should have a handle, by which it may be conveniently moved; and to each door there should be two plates, which meeting each other, and joining exactly in the middle of the door-place, may shut it very close. Each of the two plates belonging to the door of the fire-place ought to have a hole in its upper part; one of these holes should be a slit of about two lines wide, and half an inch long; the other may be a semi-circular opening of one inch in heighth and two in breadth. These holes should be placed so that neither of them may open into the fire-place when the two plates are joined together in the middle of the door to shut it close.
Fifthly, to terminate the furnace above, there must be a pyramid formed of the same materials with the furnace, hollow, quadrangular, three inches high on a base of seven inches, which base must exactly fit the upper opening of the furnace: the top of this pyramidal cover must end in a tube of three inches in diameter and two in heighth, which must be almost cylindrical, and yet a little inclining to the conical form. This tube serves, as in the furnaces already described, to carry the conical funnel, which is fitted to the upper part when a fire of extraordinary activity is wanted.
The furnace thus constructed is fit to serve all the purposes for which it is designed: yet before it can be used another piece must be provided, which, though it does not properly belong to the furnace, is nevertheless necessary in all the operations performed by it; and that is a piece contrived to contain the cupels, or other vessels which are to be exposed to the fire in this furnace. It is called a Muffle, and is made in the following manner.
On an oblong square, of four inches in breadth, and six or seven in length, a concave semi-cylinder is erected, in the form of a vault, which makes a semi-circular canal, open at both ends. One of these is almost entirely closed, except that near the bottom two small semi-circular holes are left. In each of its sides likewise two such holes are made, and the other end is left quite open.
The Muffle is intended to bear and communicate the fiercest heat; and therefore it must be made thin, and of an earth that will resist the violence of fire, such as that of which crucibles are made. The Muffle being thus constructed, and then well baked, is fit for use.
When it is to be used it must be put into the furnace by the upper opening, and set upon two iron bars, introduced through the holes made for that purpose below the door of the fire-place. The Muffle must be placed on these bars in the fire-place in such a manner that its open end shall stand next to, and directly against the door of the fire-place, and may be joined to it with lute. Then the cupels are ranged in it, and the furnace is filled up, to the heighth of two or three inches above the Muffle, with small coals not bigger than a walnut, to the end that they may lie close round the Muffle, and procure it an equal heat on every side. The chief use of the Muffle is to prevent the coals and ashes from falling into the cupels, which would be very prejudicial to the operations carrying on in them: for the lead would not vitrify as it ought, because the immediate contact of the coals would continually restore its phlogiston; or else the glass of lead, which ought to penetrate and pass through the cupels, would be rendered incapable of so doing; because the ashes mixing therewith would give it such a consistence and tenacity as would destroy that property, or at least considerably lessen it. The openings, therefore, which are left in the lower part of the Muffle, should not be so high as to admit coals or ashes to get into the cupels; the use of them is to procure an easier passage for the heat and the air to those vessels. The Muffle is left quite open in its fore-part, that the operator may be at liberty to examine what passes in the cupels, to stir their contents, to remove them from one place to another, to convey new matters into them, &c. and also to promote the free access of the air, which must concur with the fire towards the evaporation necessary to the vitrification of lead; which air, if fresh were not often enough admitted, would be incapable of producing that effect; because it would soon be loaded with such a quantity of vapours that it could not take up any more.
The government of the fire in this furnace is founded on the general principles above laid down for all furnaces. Yet as there are some little differences, and as it is very essential to the success of the operations for which this furnace is intended, that the artist should be absolutely master of his degree of heat, we shall in few words shew how that may be raised or lowered.
When the furnace is filled with coals and kindled, if the door of the ash-hole be set wide open, and that of the fire-place shut very close, the force of the fire is increased; and if, moreover, the pyramidal cover be put on the top, and the conical funnel added to it, the fire will become still more fierce.
Seeing the matters contained in this furnace are encompassed with fire on all sides, except in the fore-part opposite to the door of the fire-place, and as there are occasions which require that the force of the fire should be applied to this part also, an iron box, of the shape and size of the door, hath been contrived to answer that purpose. This box is filled with lighted coals, and applied immediately to the door-place, by which means the heat there is considerably augmented. This help may be made use of at the beginning of the operation, in order to accelerate it, and bring the heat sooner to the desired degree; or in case a very fierce heat be required; or at a time when the air being hot and moist will not make the fire burn with the necessary vigour.
The heat may be lessened by removing the iron box, and shutting the door of the fire-place quite close. It may be still further and gradually diminished, by taking off the conical funnel from the top; by shutting the door of the fire-place with one of its plates only, that which has the least, or that which has the greatest aperture in it; by taking off the pyramidal cover; by shutting the ash-hole door wholly or in part; and, lastly, by setting the door of the fire-place wide open: but, in this last case, the cold air penetrates into the cavity of the Muffle, and refrigerates the cupels more than is almost ever necessary. If it be observed, during the operation, that the Muffle grows cold in any particular part, it is a sign there is a vacuity left by the coals in that place: in this case an iron wire must be thrust into the furnace, through the hole which is over the door of the fire-place, and the coals stirred therewith, so as to make them fall into their places and fill up the vacant interstices.
It is proper to observe, that, besides what has been said concerning the ways of increasing the activity of the fire in the cupelling furnace, several other causes also may concur to procure to the matters contained in the Muffle a greater degree of heat: for example, the smaller the Muffle is, the wider and more numerous the holes in it are; the nearer to its bottom, or further end, the cupels are placed, the more will the matters therein contained be affected with heat.
Besides the operations to be performed by the cupel, this furnace is very useful, and even necessary, for many chymical experiments; such, for instance, as those relating to sundry vitrifications and enamelling. As it is pretty low, the best way is to place it, when it is to be used, on a base of brick-work that may raise it to a level with the operator's hand.
A Lamp-furnace is exceeding useful for all operations that require only a moderate, but long-continued, degree of heat. The furnace for working with a lamp-heat is very simple: it consists only of a hollow cylinder, from fifteen to eighteen inches high, and five or six in diameter, having at its bottom an aperture large enough for a lamp to be introduced and withdrawn with ease. The lamp must have three or four wicks, to the end that by lighting more or fewer of them a greater or less degree of heat may be produced. The body of the furnace must moreover have several small holes in it, in order to supply the flame of the lamp with air enough to keep it alive.
On the top of this furnace stands a bason five or six inches deep, which ought to fill the cavity of the cylinder exactly, and to be supported at its circumference by a rim which may entirely cover and close the furnace: the use of this bason is to contain the sand through which the lamp-heat is usually conveyed.
Besides this, there must be a kind of cover or dome made of the same material with the furnace, and of the same diameter with the sand-bath, without any other opening than a hole, nearly circular, cut in its lower extremity. This dome is a sort of reverberatory, which serves to confine the heat and direct it towards the body of the retort; for it is used only when something is to be distilled in a vessel of this fashion; and then the hole at its bottom serves for a passage to the neck of the retort. This dome should have an ear or handle, for the conveniency of putting it on and taking it off with ease.
_Of Lutes._
Chymical vessels, especially such as are made of glass, and the earthen vessels commonly called stone-ware, are very subject to break when exposed to sudden heat or cold: whence it comes, that they often crack when they begin to heat, and also when being very hot they happen to be cooled, either by fresh coals thrown into the furnace, or by the access of cold air. There is no way to prevent the former of these accidents, but by taking the pains to warm your vessel very slowly, and by almost insensible degrees. The second may be avoided by coating the body of the vessel with a paste or lute, which being dried will defend it against the attacks of cold.
The fittest stuff for coating vessels is a composition of fat earth, Windsor-loam, fine sand, filings of iron, or powdered glass, and chopped cow's hair, mixed and made into a paste with water. This lute serves also to defend glass vessels against the violence of the fire, and to prevent their melting easily.
In almost all distillations it is of great consequence, as hath been said, that the neck of the distilling vessel be exactly joined with that of the receiver into which it is introduced, in order to prevent the vapours from escaping into the air and so being lost: and this junction is effected by means of a lute.
A few slips of paper applied round the neck of the vessels with common size will be sufficient to keep in such vapours as are aqueous or not very spirituous.
If the vapours are more acrid, or more spirituous, recourse may be had to slips of bladder long steeped in water, which containing a sort of natural glue, close the junctures of the vessels very well.
If it be required to confine vapours of a still more penetrating nature, it will be proper to employ a lute that quickly grows very hard; particularly a paste made with quick-lime and any sort of jelly, whether vegetable or animal; such as the white of an egg, stiff size, _&c._ This is an excellent lute, and not easily penetrated. It is also used to stop any cracks or fractures that happen to glass vessels. But it is not capable of resisting the vapours of mineral acid spirits, especially when they are strong and smoking: for that purpose it is necessary to incorporate the other ingredients thoroughly with fat earth softened with water; and even then it frequently happens that this lute is penetrated by acid vapours, especially those of the spirit of salt, which of all others are confined with the greatest difficulty.
In such cases its place may be supplied with another, which is called Fat Lute, because it is actually worked up with fat liquors. This lute is composed of a very fine cretaceous earth, called tobacco-pipe clay, moistened with equal parts of the drying oil of lint-seed, and a varnish made of amber and gum copal. It must have the consistence of a stiff paste. When the joints of the vessels are closed up with this lute, they may, for greater security, be covered over with slips of linen smeared with the lute made of quick-lime and the white of an egg.
Chymical vessels are liable to be broken in an operation by other causes besides the sudden application of heat or cold. It frequently happens, that the vapours of the matters exposed to the action of fire rush out with such impetuosity, and are so elastic, that, finding no passage through the lute with which the joints of the vessels are closed, they burst the vessels themselves, sometimes with explosion and danger to the operator.
To prevent this inconvenience, it is necessary that in every receiver there be a small hole, which being stopped only with a little lute may easily be opened and shut again as occasion requires. It serves for a vent-hole to let out the vapours, when the receiver begins to be too much crowded with them. Nothing but practice can teach the artist when it is requisite to open this vent. If he hits the proper time, the vapours commonly rush out with rapidity, and a considerable hissing noise; and the vent should be stopped again as soon as the hissing begins to grow faint. The lute employed to stop this small hole ought always to be kept so ductile, that, by taking the figure of the hole exactly, it may entirely stop it. Besides, if it should harden upon the glass, it would stick so fast that it would be very difficult to remove it without breaking the vessel. This danger is easily avoided by making use of the fat lute, which continues pliant for a long time, when it is not exposed to an excessive heat.
This way of stopping the vent-hole of the receiver has yet another advantage: for if the hole be of a proper width, as a line and half, or two lines, in diameter, then, when the vapours are accumulated in too great a quantity, and begin to make a great effort against the sides of the receiver, they push up the stopple, force it out, and make their way through the vent-hole: so that, by this means, the breaking of the vessels may always be certainly prevented. But great care must be taken that the vapours be not suffered to escape in this manner, except when absolute necessity requires it; for it is generally the very strongest and most subtile part of a liquor which is thus dissipated and lost.
Heat being the chief cause that puts the elasticity of the vapours in action, and prevents their condensing into a liquor, it is of great consequence in distillation that the receiver be kept as cool as possible. With this view a thick plank should be placed between the receiver and the body of the furnace, to intercept the heat of the latter, and prevent its reaching the former. As the vapours themselves rise very hot from the distilling vessel, they soon communicate their heat to the receiver, and especially to its upper part, against which they strike first. For this reason it is proper that linen cloths, dipt in very cold water, be laid over the receiver, and frequently shifted. By this means the vapours will be considerably cooled, their elasticity weakened, and their condensation promoted.
By what hath been said in this first part, concerning the properties of the principal agents in Chymistry, the construction of the most necessary vessels and furnaces, and the manner of using them, we are sufficiently prepared for proceeding directly to the operations, without being obliged to make frequent and long stops, in order to give the necessary explanations on those heads.
Nevertheless, we shall take every proper occasion to extend the theory here laid down, and to improve it by the addition of several particulars, which will find their places in our Treatise of Chymical Operations.
ELEMENTS
OF THE
PRACTICE OF CHYMISTRY;
WHEREIN
The Fundamental Operations are described, and
illustrated by Observations on each Process.
ELEMENTS
OF THE
PRACTICE OF CHYMISTRY.
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Elements of the Theory and Practice of Chymistry, 5th ed.Chapter XXXVIII: Section III: The ANALYSIS of MINERAL SUBSTANCES (2)
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