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SECTION III.. _of Operations on The_ Semi-Metals.

Elements of the Theory and Practice of Chymistry, 5th Ed. · Pierre Joseph Macquer — chapter 40 of 43 · ~27,196 words · public domain

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Of Operations on the SEMI-METALS.

CHAP. I.

Of ANTIMONY.

PROCESS I.

To Separate Antimony from its Ore by Fusion.

Having drilled some small holes, of about two lines in diameter, in the bottom of a crucible, put into it your Antimonial Ore broken into little bits, about the size of a hazel nut; lute on its cover; set the crucible thus prepared in the mouth of another crucible, and close the joints with lute.

At the distance of half a foot from this compound vessel place bricks all round, so as to form a furnace; the sides of which must rise as high as the brim of the uppermost crucible.

Let the bottom of this furnace be filled with ashes, up to the top of the lower crucible, and the rest of the furnace with lighted coals. Blow the fire, if it be necessary, with bellows, till the upper crucible become red. Keep it up in this degree for about a quarter of an hour. Then take your vessels out of the furnace, and you will find the Antimony collected in the bottom of the lower crucible, having run through the holes of the upper one.

OBSERVATIONS.

The ore of Antimony is one of the most fusible: it always contains a great deal of Sulphur, and cannot sustain a fire of any force without being dissipated into vapours. It requires no additament to flux it: for it is not necessary, on this occasion, that the earthy and stony matters mixed therewith be brought to fusion. It is sufficient that the Antimonial part be melted; which, as soon as it becomes fluid, is carried by its weight to the lower part of the crucible. Thus it is separated from all heterogeneous matters; which are left in the upper crucible, while it passes through the holes in its bottom, and forms a mass in the lower.

The precaution of closing all the apertures of both crucibles is necessary, on account of the volatility of this mineral: and that the Antimony, when once melted, may not continue exposed to a great heat, it is made to run down into a vessel surrounded with ashes only, and by that means very little affected with heat; ashes being one of those solid mediums that transmit least of it.

PROCESS II.

The common Regulus of Antimony.

Reduce crude Antimony to powder. Mix it with three fourths of its weight of white Tartar, and half its weight of refined Salt-petre, both pulverized. Into a large crucible made red-hot in the fire, throw a spoonful of your mixture, and cover it. There will be a very considerable detonation. When it is over, throw in a second spoonful of your mixture, and cover the crucible as before: this will produce a second detonation. Go on thus, till you have thrown in all your mixture.

When the whole has thus fulminated, increase the fire so as to bring the matter into fusion; that being done, take the crucible out of the furnace, and immediately pour its contents into an iron cone heated and greased with tallow. Strike the floor and the cone some gentle blows with a hammer, to make the Regulus precipitate: and when the matter is fixed and cold, invert the cone and turn it out. You will see it consist of two distinct substances; the uppermost of which is a saline scoria, and the undermost the reguline part. Strike this mass a blow with a hammer, in the place where these substances join, and you will by this means separate the scoria from the Regulus; the latter of which will have the form of a metallic cone, on whose base you will observe the signature of a bright star.

OBSERVATIONS.

Antimony, though separated by a former fusion from the earthy and stony parts of its ore, must nevertheless be still considered as an ore, on account of the great quantity of Sulphur it contains, which mineralizes the metalline part or Regulus. Therefore, if you desire to have this Regulus pure, you must separate it from the Sulphur that is combined with it. This may be done several ways. The method above proposed is one of the readiest and easiest, though not altogether free from inconveniencies, as we shall shew.

The Salt-petre in the mixture detonates by means of the Sulphur of the Antimony, which it consumes, and from which it separates the reguline part: but lest it should also consume some of the phlogiston which gives the Regulus its metalline form, Tartar is added; because it contains a great deal of inflammable matter, and so is capable of furnishing enough for the detonation of the Nitre, or rather for restoring to the metallic earth of the Antimony, the phlogiston that may be consumed by the Nitre.

If we consider what passes in this operation we shall soon be convinced that a great deal must be lost in it, and that we do not thereby obtain near the whole of the Regulus that the Antimony is capable of yielding: for, 1. the Regulus of Antimony being a volatile substance, much of it must be dissipated during the detonation; and so much the more as the detonation is frequently repeated, and continued for a considerable time. The flowers that may be collected by presenting cold bodies to the smoke that rises in the operation, and which may be reduced to a Regulus by the addition of a phlogiston, sufficiently prove what is here advanced.

2. All the Sulphur of the Antimony is not consumed by the Nitre on this occasion; and moreover, the Acid of that part thereof which is burnt, uniting with some of the Alkali produced by the deflagration of the Nitre and Tartar, forms a Vitriolated Tartar, which meeting with a sufficient quantity of phlogiston in the mixture produces new Sulphur. Now this Sulphur, whether not consumed, or reproduced, in the operation, combining with the Alkali forms a Liver of Sulphur; and that dissolves part of the Regulus, which by this means remains confounded with the scoria. The proof of this is, that, if the scoria be mixed with filings of iron, and fused a second time, you will find at the bottom of the crucible a button of Regulus, which it contained, and which is separated therefrom by the interposition of the Iron. We shall say more on this subject in the process for making the Martial Regulus, which immediately follows this. If, instead of melting the scoria with iron filings, we pulverize it, boil it in water, and then pour an acid into that water; the liquor will instantly grow turbid, and a Sulphureous Precipitate will fall, commonly called the Golden Sulphur of Antimony; which is nothing else but common Sulphur still combined with some particles of the Regulus; a new proof of what we advanced concerning the production of Liver of Sulphur in this operation.

As Regulus of Antimony is of no great value, the loss sustained in this process is seldom regarded. However, we shall have occasion, in the sequel, to point out a method of obtaining this Regulus with less disadvantage.

PROCESS III.

Regulus of Antimony precipitated by Metals.

Put one part of small iron nails into a crucible, and set it amidst burning coals, in a melting furnace. When the iron is thoroughly red-hot, and begins to grow white, add thereto little by little, and at several times, two parts of crude Antimony in powder. The Antimony will immediately flow and unite with the Iron. When the Antimony is entirely melted, add thereto, at several times, the fourth of its weight of pulverized Nitre: a detonation will ensue, and the whole mixture will be in fusion.

After you have kept the matter in this condition for some minutes, pour it into an iron cone, first heated and tallowed. Strike the sides of the cone with a hammer, that the Regulus may fall to the bottom; and, when all is cold, separate it from the scoria by a blow with a hammer. Melt this first Regulus again in another crucible, adding a fourth part of its weight of crude Antimony. Keep the crucible close shut, and give no more heat than is necessary to melt the matter. When it is in perfect fusion, add to it at several times, as you did before, the sixth part of its weight of pulverized Nitre; and, in half a quarter of an hour after this, pour the whole into a cone as you did the first time.

Lastly, melt your Regulus over again a third, or even a fourth time, always adding a little Nitre, which will detonate as before. If after all these fusions you pour the Regulus into an iron cone, you will find it very beautiful, and the star well formed: it will be covered with a semi-transparent, lemon-coloured scoria. This scoria is extremely acrid and caustic.

OBSERVATIONS.

Though Regulus of Antimony unites very readily with Sulphur, and is always found combined therewith in the earth, we must not thence conclude that it hath a greater affinity than other substances with that mineral: on the contrary, all the metals, except Gold, have a greater affinity than this Semi-metal with Sulphur. Hence it follows that all the metals, except Gold, are capable of decomposing Antimony, and separating the sulphureous part from the metalline; so that, instead of employing Iron, as in our process, Copper, Lead, Tin, or Silver, may be used, and a Regulus obtained by means thereof.

But as Iron is, of all the metallic substances, that which hath the greatest affinity with Sulphur, it is on this occasion preferred to the rest. And from hence two advantages arise: the first is, that the operation is performed sooner and with greater ease: the second, that the Regulus is purer, and contains less of the precipitating metal. For it is a general rule, that, when one metallic substance is employed to precipitate another, the precipitated substance is always a little adulterated by the admixture of some particles of the precipitant. Now, the greater affinity the precipitant hath with the matter united to that which is to be precipitated, the less doth the precipitate retain of the precipitant.

In this process the Iron melts very easily by means of the union it contracts with the Sulphur; which, as we observed before, hath the property of rendering this metal very fusible, though of itself the most refractory of all.

The scoria found on the Regulus of the first fusion is a combination of Iron with the sulphureous part of the Antimony. This scoria is extremely hard, and not to be separated from the Regulus without some trouble. The Nitre added, being alkalizated and united therewith, renders it a little softer, and gives it the property of relenting in the air. Any Alkaline Salt may be substituted for the Nitre.

The Nitre that is alkalizated in the operation, or the Alkali that is added, procures moreover another advantage; namely, that, by uniting with part of the Sulphur of the Antimony, it produces a Liver of Sulphur, which dissolves the Iron, retains it, and hinders that which is not yet combined with pure Sulphur from uniting so readily with the Regulus as it otherwise would do.

Lastly, the addition of Nitre, or an Alkali, contributes greatly to promote the fusion, to render it more perfect, and to procure a more complete precipitation of the Regulus.

The second fusion which the Regulus is made to undergo is intended to purify it from any mixture of Iron. When the fresh Antimony added on that occasion comes to melt with the Regulus, the Sulphur contained in the Antimony joins with the ferruginous parts in the Regulus; and the Iron becoming lighter by this union is thrown up to the surface of the matter. There it forms a sort of scoria, with which a good deal of Antimony is mixed; the Regulus not being wholly precipitated, because there is not Iron enough in the mixture for that purpose. The Salt-petre added here produces the same effect as in the first fusion.

But if, on one hand, the Regulus precipitated in the first fusion be purified, by this addition of fresh Antimony, from most of the Iron with which it was alloyed; on the other hand, this same Regulus cannot be kept from re-uniting with some sulphureous parts.

In order therefore to separate it entirely from these, it must be melted over again once or twice more, and a little Nitre added each time, to consume them by deflagration. But this cannot be done without consuming also some of the very phlogiston which gives the Regulus its metalline form: whence it comes to pass that part of the Regulus is converted to a calx, which, by means of the alkalizated Nitre, is turned into glass; and it is this glass which mixing with the scoria gives it the yellow colour observed therein. This yellow colour may also be in part produced by some ferruginous particles, of which a small quantity always remains combined with the Regulus, notwithstanding its former depuration by Antimony.

It is of no use to repeat the fusions of the Regulus oftener than is above proposed, or to add fresh Nitre with a view to consume the Sulphur it may still contain: for after the second fusion it contains none at all, and retains only the phlogiston necessary to give it the metalline form. So that, by prosecuting the matter further, you would only calcine and destroy the Regulus to no manner of purpose.

From what hath been said it is plain that, even by this process, we do not obtain all the Regulus which our Antimony is capable of yielding; seeing part of it is destroyed by the fusions it must necessarily undergo with Nitre, in order to its purification. We shall give a process for obtaining from Antimony the greatest quantity of Regulus it can possibly be made to yield, after we have treated of its Calcination, which is in some sort the first step of that process.

PROCESS IV.

The Calcination of Antimony.

Take an unglazed earthen vessel, wider at top than at bottom; put into it two or three ounces of crude Antimony finely pulverized. Set this vessel over a weak charcoal fire, and increase the heat till you see the Antimony begin to smoke a little. Continue the fire in this degree, and keep incessantly stirring the Antimony with the shank of a tobacco-pipe all the while it is upon the fire.

The powder of Antimony, which, before calcination, was of a brilliant colour inclining to black, will become dull, and look like an earth. When it comes to have this appearance raise your fire till the vessel be red-hot, and keep it up in this degree till the matter cease entirely to smoke.

OBSERVATIONS.

Antimony, as hath been already said, is a sort of ore consisting of a metalline or reguline part mineralized by Sulphur.

The design of this calcination is, by the action of fire, to dissipate the sulphureous part, which is the most volatile, in order to separate it from the metalline part. It is evidently a real torrefaction; but the operation is very difficult, and requires a good deal of attention; for Antimony very easily melts, while at the same time it is necessary to our success that it do not melt; because when the matter is in fusion the Sulphur requires a much greater degree of heat to carry it off. Now, as Regulus of Antimony itself is very volatile, a good deal of it would be dissipated along with the Sulphur, if it were exposed to the degree of heat necessary to carry off the Sulphur when the mass is melted.

Therefore if it happen that the Antimony begin to melt during the calcination, which is easily perceived by its running into clots, it must be taken off the fire, and the clotted parts be again pulverized; after which the calcination is to be prosecuted with a less degree of heat.

When the Antimony has lost all its brightness, and is become like an earth, it is time to augment the degree of heat, in order to complete the calcination; because the last portions of the Sulphur are the most difficult to raise. Moreover, the inconveniences just mentioned are not now to be apprehended: for, as the great fusibility of the reguline part is owing to the Sulphur, what remains, after you have dissipated the greatest part of the Sulphur, is much less fusible; and, as the redundant Sulphur of the Antimony cannot be driven off, without dissipating at the same time a good deal of the phlogiston necessary to metallize its Regulus, the matter that remains comes much nearer to the nature of a calx, than to that of a metalline substance; and consequently partakes of the nature of all metallic calces, which is to be very fixed.

Antimony may also be calcined by mixing with that mineral an equal quantity of charcoal-dust. As charcoal is incapable of fusion, it prevents the Antimony from clotting, as well as from losing so much of its metallizing phlogiston as it otherwise would: and hence it comes to pass that the calx of Antimony, prepared in this manner, comes nearer to the nature of a Regulus, than that which is prepared without addition.

If you happen to raise the fire too much, in this calcination with charcoal-dust, the calx will be partly reduced to a Regulus, by means of the phlogiston which the charcoal furnishes; and then the Regulus will be dissipated in vapours, especially as this calx, which comes very near the nature of a Regulus, is not so fixed as that prepared without addition. For this reason it always continues to smoke, even when it contains no superfluous Sulphur: and therefore you must not wait till it cease to smoke before you put an end to your calcination; for you will lose a great deal of it in vapours. It is time to stop when the vapours that rise from it, while it is moderately red, do not smell of burning Sulphur.

PROCESS V.

Calx of Antimony reduced to a Regulus.

Mix the calx of Antimony, which you intend to reduce, with an equal quantity of black soap. This mixture will make a thin paste. Put it little by little into a crucible, previously made red-hot amidst live coals. Thus let the soap burn till it cease to emit any oily smoke. Then cover the crucible; make the fire strong enough to melt the matter, and you will hear it effervesce and boil. When this noise is over let the crucible cool, and then break it: you will find in it a beautiful scoria, marked with circles of several colours; and under that a button of Regulus, which is not yet quite pure, and must be purified in the following manner.

Pound this Regulus, and mix it with half its weight of an antimonial calx as perfectly desulphurated as possible. Put it into a crucible, and cover it: melt the whole, so that the surface of the melted matter may be smooth and uniform. Let the crucible cool, and then break it: you will find in it a beautiful button of very pure Regulus, covered with a scoria having the appearance of an opaque glass, or a kind of greyish enamel, moulded on the finely radiated surface of the Regulus.

OBSERVATIONS.

Of all the metalline calces that of Antimony is most easily reduced. Any matter that contains the phlogiston, even charcoal-dust alone, is sufficient to procure it the form of a Regulus, without the addition of any thing to facilitate its fusion; because this calx, which is not of itself altogether refractory, becomes still more fusible as it combines with the phlogiston, and approaches to the reguline state.

Though all inflammable matters are capable of procuring the reduction of the calx of Antimony, yet there are some with which the operation succeeds better, and produces a greater quantity of Regulus, than it does with others. Fatty matters, joined with Alkalis, are those which answer best in this reduction, as they do in most others. The black flux, for instance, is very proper for this purpose: but Mr. Geoffroy, who made many experiments on Antimony, found by repeated trials that black soap is still fitter for it, and that a greater quantity of Regulus was obtained by its means, than by any other reducing flux whatever. The process here given is taken from one of the Memoirs on this subject, which he laid before the Academy of Sciences.

Black soap is made of the lye of a Fixed Alkali, such as potash for instance, with quick-lime, incorporated by boiling with oil of lint-seed, rape-seed, or hemp-seed, and sometimes also with animal fat. The oily matters, contained in this reducing flux, are first burnt and charred to a coal in the crucible. As soon as they are brought to this state, the crucible is covered, and the fire is increased, till the matters melt. At that instant the reduction begins to take place; and the bubbling noise observed is an effect thereof.

The Regulus obtained by this first fusion is not yet very pure, being adulterated with the mixture of some unmetallic earth that was contained in the Antimony, and with a portion of the calcarious earth of the soap.

Mr. Geoffroy found that his Regulus was contaminated with this substance, by putting it into water: for on that occasion he observed a very brisk ebullition about the reguline buttons, which sometimes lasted above four and twenty hours; and on examining them with a glass, he discovered some little holes, imperceptible to the naked eye, through which the water entered, to unite with the lime retained in the internal parts of the Regulus, which having been recalcined in the operation required to be slaked.

This Regulus may be purified by simple fusion, without any additament, because the particles of lime, being lighter than those of the Regulus, will be thrown up to the surface, on which they will form a sort of scoria. But Mr. Geoffroy took notice that, in this case, the surface of the Regulus is never very neat; that it is always sullied with a very adhesive scoria, and that no star is formed upon it. Besides, the Regulus must be kept a long while in very thin fusion, that the heterogeneous matters, which hinder the perfect re-union of its parts, may have time to rise to the surface by their lightness. But the longer the Regulus is kept in fusion, the more of it evaporates, because of its volatility. He was therefore obliged to have recourse to other means.

We have in the process described the method which succeeded best with Mr. Geoffroy. It consists in melting the Regulus over again, with the addition of a little fresh calx of Antimony thoroughly freed from its Sulphur. This calx being in its nature easily vitrifiable, and combining with the earthy parts that deprave the Regulus, and which cannot be vitrified without addition, scorifies these matters, and with them forms the opaque glass, or kind of enamel which is found over the Regulus purified in this manner.

The star on that part of the Regulus of Antimony, which was contiguous to the scoria, is a mark of its purity, and a proof that the operation was well performed. This star is nothing but a particular disposition of the parts of the Antimony, which have the property of running naturally into facets and needles. The perfect fusion, both of the Regulus and the scoria that covers it, leaves the parts of the Regulus at liberty to range themselves in this order. This disposition appears not only on the upper surface of the Regulus, but, if you break the button, you find the same in its internal parts. There are some round pyrites whose insides have nearly the same appearance, and seem to consist of rays issuing from a common center.

The quantity of Regulus obtained by Mr. Geoffroy's process is more than double of what is procured in the common way, which yields but about four ounces in the pound; whereas this gives from eight to ten ounces.

When Antimony is calcined with charcoal-dust, what remains after the dissipation of all the Sulphur is not, properly speaking, a calx of Antimony; but a sort of Regulus quite formed, and differing from the common Regulus only in that its parts are disunited, and not collected into a mass. For if this pretended calx of Antimony be melted, it directly coalesces into a Regulus, without the addition of any inflammable matter fit to procure its reduction. Indeed less Regulus is obtained by this means than when a reductive is added: but nevertheless this experiment still proves what I advanced; seeing Regulus of Antimony cannot be melted without losing more or less thereof, either because some of it is dissipated in vapours, or because part of it loses its phlogiston in the fusion, and so is converted into a calx.

PROCESS VI.

Antimony calcined with Nitre. Liver of Antimony. Crocus Metallorum.

Pulverize and mix perfectly together equal parts of Nitre and Antimony: put the mixture into an iron mortar, and cover it with a tile, which however must not shut it quite close. With a live coal set fire to the matter in the mortar, and immediately withdraw it. The mixture will flame, with great detonation; which being over, and the mortar cooled, invert it, and strike its bottom to make all the matter fall out. Then, by a blow with a hammer, separate the scoria from the shining part, which is the Liver of Antimony.

OBSERVATIONS.

In this operation the Nitre takes fire and detonates with the Sulphur of the Antimony; and nothing remains but the metallic earth of the mineral, which, meeting with no substance to restore its phlogiston, cannot take the form of a Regulus; but, being combined with a large quantity of fused saline matters, begins itself to flow, and forms a sort of vitrification; which, however, is not a complete one, because the matters do not continue long enough in fusion, but cool too soon. This preparation of Antimony is a violent Emetic. It is used to make Emetic Wine and Tartar Emetic: it is also given in substance to horses.

The saline matters found after the operation in the form of a scoria, or perhaps confounded with the Liver of Antimony, are combinations of Fixed Nitre, partly with the Acid of the burnt Sulphur, forming a Neutral Salt of the same kind as Vitriolated Tartar, and partly with some unburnt Sulphur, forming a sort of Liver of Sulphur that contains a little Regulus. It is usual to pulverize this Liver of Antimony and wash it with water, in order to dissolve and carry off all the Salts. When thus pulverized and washed it is called Crocus Metallorum. If Liver of Antimony be melted with any inflammable matter, it will be reduced to a Regulus; because it is nothing but a metalline calx half vitrified.

PROCESS VII.

Another Calcination of Antimony with Nitre. Diaphoretic Antimony. Materia Perlata. Clyssus of Antimony.

Mix one part of Antimony with three parts of Nitre; project this mixture by spoonfuls into a crucible kept red-hot in a furnace. Each projection will be attended with a detonation. Continue doing this till you have used all your mixture: then raise the fire, and keep it up for two hours; after which throw your matter into a pan full of hot water. Let it lie steeping in water kept hot for a whole day. Then pour off the liquor: wash the white powder you find at bottom in warm water; and repeat the ablutions till the powder become insipid. Dry it, and you have Diaphoretic Antimony.

OBSERVATIONS.

This operation differs from the preceding one, in respect of the quantity of Nitre deflagrated with the Antimony. In the former we added one part only of Nitre to one part of Antimony; but in this three parts of Nitre are put to one of the mineral; and the calx resulting from this mixture is of course very different from the other.

In the first place, Liver of Antimony hath a reddish colour; whereas Diaphoretic Antimony is very white. Secondly, Liver of Antimony is in a manner half vitrified; Diaphoretic Antimony is, on the contrary, in the form of a powder, the parts of which have no connection together.

The reason of these differences will easily appear, if we consider, that, Liver of Antimony being the result of calcination with one part of the Nitre only, which is not sufficient to consume all the Sulphur of the mineral, what remains after the detonation is not entirely deprived of its phlogiston; from whence arise the colour it retains and the ease with which it flows in the fire: but that, when three parts of Nitre are added instead of one, this quantity is not only sufficient to consume all the Sulphur and the phlogiston of the Antimony, but even more than enough; seeing that, after the operation, some Nitre is still found undecomposed.

The calx of Antimony, prepared by calcining it with three parts of Nitre, is therefore deprived of all its phlogiston. This is the cause of its whiteness, and the reason why it is not half vitrified by the operation, as Liver of Antimony is: for we know that the more a metallic calx is deprived of its phlogiston, the less fusible and the less vitrifiable it is. This calx of Antimony bears the name of Diaphoretic Antimony, or Diaphoretic Mineral: because, being neither emetic nor purgative, it is thought to have the virtue of promoting perspiration.

Antimony may be calcined with various proportions of Nitre, between that used to make Liver of Antimony, and this with which Diaphoretic Antimony is prepared; and from these calcinations will result calces possessed of properties both chymical and medical, of an intermediate nature between the extremes of those two preparations. The nearer the proportion of Nitre comes to that employed in preparing Liver of Antimony, the more will the resulting calx resemble that preparation; and in the same manner, a calx prepared with a greater proportion of Nitre will so much the more resemble Diaphoretic Antimony, as the proportion of Nitre used comes nearer three parts of Nitre for one of Antimony.

It is not necessary that Antimony in substance be employed to make the Diaphoretic Mineral: you may, if you please, make use of its Regulus. But as the Regulus contains no Sulphur, nor any more phlogiston than is requisite to secure its metalline form, it is needless to put three parts of Nitre to one of Regulus; an equal quantity thereof being sufficient.

The matter is projected by spoonfuls, to the end that, by gradual and repeated detonations, the Antimony may be more perfectly calcined: it is also with a view to destroy entirely the small remainder of phlogiston, which may have escaped the action of the Nitre, that the matter is kept red-hot in the crucible for two hours.

The whole is afterwards thrown into hot water, and left steeping therein for several hours, with design to give the water time to dissolve all the saline matters that are mixed with the Diaphoretic Calx. When crude Antimony is used in making this preparation, these saline matters are, 1. an Alkalizated Nitre; 2. a Neutral Salt formed by the union of the Acid of Sulphur with part of that Alkali, as in the preparation of Liver of Antimony; 3. a portion of undecomposed Nitre.

The water in which the Diaphoretic is washed takes up moreover a portion of the calx of Antimony, which is exceeding finely attenuated, and continues united with the fixed Nitre, and suspended therewith in the liquor. This matter is to be separated from the Fixed Nitre, by mixing the water wherein it is dissolved with an Acid, which unites with the Alkali, and precipitates this matter in the form of a white powder, to which the name of Materia Perlata hath been given. Because it is precipitated in the same manner as the Golden Sulphur of Antimony, and, like that, is found in the water with which the saline matters are washed out, after the detonation of Nitre with Antimony, some Chymists have given it, though very improperly, the name of the Fixed Sulphur of Antimony.

This matter is a true Calx of Antimony, and differs from Diaphoretic Antimony in nothing but its being still more perfectly calcined. It is so indeed to such a degree that it is impossible to restore its metalline form, or reduce it to a Regulus, by the addition of an inflammable matter. Diaphoretic Antimony, on the contrary, may be re-metallized, by supplying it with phlogiston: but it must be observed that, in whatever manner you go about this, you will obtain a much smaller quantity of Regulus, than when you use a Calx of Antimony prepared with a smaller quantity of Nitre.

If you attempt to reduce either Liver of Antimony or Diaphoretic Antimony, great care must be taken to wash them thoroughly, in order to free them from every thing saline: for, without this precaution, the Acid of the Sulphur, having, as was observed, formed a Neutral Salt with the Alkali of the Nitre, will combine with the inflammable matter added to revivify the calx of Antimony and reproduce a Sulphur; which, uniting afterwards with the same Alkali, will produce a Liver of Sulphur, that will dissolve part of the Regulus, hinder its precipitation, and greatly lessen the quantity which might otherwise be expected.

A particular sort of Diaphoretic Antimony is sometimes prepared for Medical uses, which hath a purgative quality: it is not washed at all, and is therefore called Unwashed Diaphoretic Mineral.

Diaphoretic Antimony may also be prepared in close vessels, by means of which the vapours that rise during the operation are retained. For this purpose a tubulated retort is employed, having a series of adopters fitted to it. The retort is placed in a furnace, and heated till its bottom become red: then a very small quantity of the mixture, for making Diaphoretic Antimony, is introduced through the tube in the upper part of the retort, and the tube immediately stopped. A detonation ensues, and the vapours expand themselves into the adopters, where they condense. This is repeated till the intended quantity of matter be used. After the operation some white flowers are found sublimed in the neck of the retort, and a small quantity of liquor in the recipients. This liquor is acid. It consists of some of the Acid of the Nitre, which the Acid of the Sulphur hath expelled from its basis, and also a little of the Acid of the Sulphur carried up by the heat before it could combine with the basis of the Nitre. This liquor is called Clyssus of Antimony. The name of Clyssus is given to all liquors in general that are prepared by this method.

The white flowers found in the neck of the retort are flowers of Antimony; that is, a calx of Antimony forced up by the heat, and by the impetus of the detonation. These flowers may be reduced to a Regulus. What remains in the retort is the same with the matter that remains in the crucible, wherein the mixture of Nitre and Antimony for making Diaphoretic Antimony hath been deflagrated.

Neither Diaphoretic Antimony nor the Pearly matter are soluble in any Acid.

PROCESS VIII.

Calx of Antimony Vitrified.

Take any quantity you please of calx of Antimony, made without addition; put it into a good crucible, which set in a melting furnace: kindle the fire gradually, and leave the crucible uncovered at the beginning.

A quarter of an hour after the matter is red-hot, cover the crucible, and excite the fire vigorously till the calx melt. You may know when it is thoroughly melted, by dipping into the crucible an iron wire, to the end of which a little knob of glass will adhere, if the matter be in perfect fusion. Keep it in fusion for a quarter of an hour, or rather longer if your crucible can bear it. Then take it out of the furnace, and immediately pour out the melted matter on a smooth stone, made very hot for the purpose: it will presently fix into a yellow Glass.

OBSERVATIONS.

All the calces of Antimony, when exposed to a violent fire, are converted into Glass; but not all with the same facility. In general, the more of their phlogiston they have lost in the calcination, the more difficult is their vitrification. This causes also a difference in the colour of the Glass; which will be of so much a deeper yellow, and the nearer to a red, the less the Antimony was calcined.

It frequently happens, when we employ a calx of Antimony which is not sufficiently deprived of its phlogiston, that we find in the crucible a button of Regulus, which, being heavier than the Glass, always lies at the bottom. With a view to avoid this inconvenience, and to dissipate completely the excess of phlogiston that may still be left in the calx of Antimony, we direct the crucible to be left uncovered for some time, at the beginning of the operation. If, notwithstanding this precaution, any Regulus be still found at the bottom of the crucible, and you resolve to vitrify it, the crucible must be returned to the furnace, and the fusion continued; by which means the Regulus will at last be converted into Glass.

If, on the contrary, you meet with any difficulty in effecting the vitrification, on account of your having employed a calx that hath lost too much of its phlogiston, such as Diaphoretic Antimony, or the Pearly matter, the fusion may be greatly facilitated by throwing into the crucible a little crude Antimony.

Glass of Antimony is a most violent emetic. This Glass, as well as Liver of Antimony, is employed in preparing Emetic Wine and Emetic Tartar.

It may be resuscitated, like the calces of Antimony, into a Regulus, by re-uniting it with a phlogiston. For this purpose it must be finely pulverized, thoroughly mixed with some black flux, and melted in a covered crucible. This Glass, as well as that of Lead, hath the property of greatly promoting the vitrification of matters that are to be scorified.

PROCESS IX.

Kermes Mineral.

Break any quantity you will of Hungarian Antimony into little bits: put it into a good earthen coffee-pot: pour on it twice its weight of rain-water, and a fourth part of its weight of well filtered liquor of Nitre fixed by charcoal. Boil the whole briskly for two hours, and then filter the liquor. As it cools it will acquire a red colour, grow turbid, and leave a red powder on the filter.

Return your Antimony into the coffee-pot. Pour on it as much rain-water as before, and three fourths of the former quantity of the liquor of Fixed Nitre. Boil it again for two hours, and then filter the liquor. It will again deposite a red sediment. Return your Antimony into the coffee-pot: pour on it the same quantity of rain-water, and half the first quantity of the liquor of Fixed Nitre. Boil it again for two hours, and then filter the liquor as formerly. Wash all these sediments with warm water, till they become insipid; then dry them, and you have the Kermes Mineral.

OBSERVATIONS.

If you recollect what we said concerning the property which Fixed Alkalis possess of uniting with Sulphur, both by fusion, and, when those Salts are resolved into a liquor, by boiling, and of forming therewith a Liver of Sulphur, which dissolves all metalline substances, you will readily comprehend the nature of this Kermes.

Antimony consists of a sulphureous and a reguline part. Therefore, if this mineral be boiled in a solution of a Fixed Alkali, such as Nitre fixed by charcoal, the Alkali will dissolve the Sulphur of the Antimony, and form therewith a Liver of Sulphur, which, in its turn, will dissolve the reguline part. Now, Kermes Mineral, prepared as above directed, is no other than a Liver of Sulphur combined with a certain quantity of Regulus of Antimony.

Mr. Geoffroy hath set this truth in the clearest light, by his accurate analysis of the Kermes Mineral. The experiments he made on that subject are circumstantially related in several Memoirs printed in the volumes of the Academy for 1734 and 1735. By combining Acids with the Kermes he demonstrated, 1. the existence of Sulphur in this compound; having separated from it a burning Sulphur, which cannot be mistaken for any other than the Sulphur of Antimony. In order to obtain this Sulphur pure, an Acid must be employed that will not only absorb the Alkali, but also perfectly dissolve the reguline part that might otherwise remain united with the Sulphur. Aqua regia was the Acid which succeeded best with Mr. Geoffroy. 2. He also proved that there is a Fixed Alkali in the composition of the Kermes; seeing the Acids with which he precipitated the Sulphur became Neutral Salts, and just such as those very Acids combined with a Fixed Alkali would have constituted: that is, the Vitriolic Acid produced a Sal de duobus; the Nitrous Acid a regenerated Nitre; and the Marine Acid a regenerated Sea-salt. 3. Mr. Geoffroy demonstrated the reguline part of Antimony to be an ingredient in the Kermes; having procured therefrom an actual Regulus of Antimony, by fusing it with the black flux.

In preparing the Kermes it is necessary to renew the liquor from time to time, as above directed; because, when it is once impregnated with Kermes to a certain degree, it can take up no more; and consequently the same liquor cannot operate again on the Antimony. Experience hath shewn, that, if the doses above prescribed be applied, the liquor will after two hours boiling be sufficiently saturated with Kermes.

If the liquor in which the Kermes is dissolved be filtered while it is very hot, and almost boiling, it leaves nothing on the filter; the Kermes passing through with it: but as it cools it grows turbid, and gradually deposites the Kermes. Therefore it ought not to be filtered till it be cold; or, if it be filtered while it is boiling hot, in order to separate from it some coarse particles of Antimony not yet converted into Kermes, it must be filtered a second time when it is cold, in order to get the Kermes.

Though in the method usually practised for making Kermes, the Antimony is boiled only thrice, yet it does not follow that more Kermes may not be obtained from it, or that but little more would be obtained by a fourth and fifth boiling; on the contrary, it would yield considerably more. Mr. Geoffroy observed, that he got more Kermes by the second boiling than by the first, and still more by the third than by the second; and that the yield goes on increasing in this manner to a very great number of times, which he hath not determined. This increased effect arises from hence, that by multiplying the frictions of the little bits of Antimony against each other, new surfaces are exposed to the action of the Alkaline liquor, and furnish it with more Sulphur; while the addition of this sulphur renders the hepar more active and more penetrating; or, if you please, produces a new hepar every time the matters are boiled. When the Alkaline liquor is once saturated with Kermes, it ceases to act, and forms no new hepar; but it does not follow that its virtue is quite exhausted. To restore its ability of acting as well as at first, or nearly so, you need only let it cool, and deposite the Kermes dissolved in it. We owe this singular observation also to Mr. Geoffroy: he had the patience to go through no less than threescore and ten boilings with the same liquor, without adding any thing but rain water, to supply the place of what was dissipated by evaporation: and he always obtained a pretty considerable quantity of Kermes by each boiling, for the reason given above.

Boiling is not the only means of making Kermes. Mr. Geoffroy found the way of making it by fusion. For this purpose you must mix accurately one part of very pure Fixed Alkali, dried and pulverized, with two parts of Hungarian Antimony also pulverized, and melt the mixture. Mr. Geoffroy made use of a retort. When the mass is melted, it must again be pulverized, while it is still hot, and then put into, and kept in, boiling hot water for an hour or two; after which the liquor, now become saline and antimonial, must be filtered into another vessel filled with boiling water. Every ounce of Antimony treated in this manner yields, by thrice boiling the melted mass, from six drams to six drams and a half of Kermes; which differs from the Kermes made by boiling, only in that it is not quite so soft to the touch, having in every other respect the same qualities.

As Liver of Sulphur is made two different ways, to wit, by boiling and by fusion, and as the Kermes is nothing but a Liver of Sulphur in which the reguline part is dissolved; it follows that Kermes may be made by fusion as well as by boiling. It is necessary to pulverize the melted mass, and to steep it in boiling hot water for an hour or two, that the water may dissolve and divide it sufficiently to make the Kermes fine and beautiful.

With the same view, that is, to make it finer and more perfect, Mr. Geoffroy orders the water saturated with the Kermes made by fusion, to be received, when filtered, in a vessel full of other boiling hot water. He observed, that when the liquor impregnated with Kermes cools too fast, the Kermes that precipitates is much coarser. The warm solution of Kermes is diffused through the boiling-hot water into which it is filtered, and is thereby enabled to retain its heat so much the longer.

From what hath been said on the nature of Kermes, it plainly appears that there must be a great resemblance between it and the Golden Sulphur of Antimony, obtained from the scoria, either of plain Regulus of Antimony, or of the Liver of Antimony; this Golden Sulphur being no other than a portion of the Antimony combined with the Nitre alkalizated during the operation.

Yet there is a difference in the manner of precipitating these two compounds: for the Kermes precipitates spontaneously, on the bare cooling of the water in which it is dissolved; whereas an Acid is employed to precipitate the Golden Sulphur suspended in the water, with which the scoria of the plain Regulus of Antimony, or that of Liver of Antimony, hath been washed. This gives some ground to suspect that the reguline part is not so intimately united with the Liver of Sulphur in the Kermes, as in the scoriæ from which the Golden Sulphur is obtained.

PROCESS X.

Regulus of Antimony dissolved in the Mineral Acids.

Compound an aqua regis by mixing together four measures of Spirit of Nitre, and one measure of Spirit of Salt: on a sand-bath moderately heated place a matrass, into which pour sixteen times as much of this aqua regis as you have Regulus to dissolve. Break your Regulus into little bits; and throw them successively one after another into the matrass, observing not to add a new one till that put in before is entirely dissolved: continue this till your Regulus be all used. By degrees, as the dissolution advances, the liquor will acquire a beautiful golden colour; which, however, will insensibly disappear, as the white fumes that continually ascend from it evaporate.

OBSERVATIONS.

Regulus of Antimony is one of those metalline substances that dissolve with the greatest difficulty. Not but that most of the Acids attack and corrode it; but they do not make a clear, limpid solution thereof: they in some sort only calcine it, and this semi-metal, as fast as it dissolves, precipitates of its own accord in the form of a white magistery. In order to effect a complete dissolution thereof, it is necessary to employ an aqua regis compounded as directed, and in the dose prescribed in the process, which is wholly taken from Mr. Geoffroy's Memoirs on Antimony mentioned above.

If, instead of the Regulus, small bits of crude Antimony be thrown into the aqua regis, the Acid will attack and dissolve the reguline part, and so separate it from the sulphureous part which it will not touch. When the dissolution is finished, the particles of Sulphur being now become lighter, because no longer united with the metalline part, will float upon the liquor. Being collected they form a true Sulphur, which seems no way different from common brimstone. This operation, you see, is a sort of Parting Process.

The Vitriolic Acid, whether concentrated or much weakened with water, does not act when cold either on Antimony or on its Regulus. This Acid only dims the splendour of the facets of the Regulus; but if one part of exceeding pure Regulus of Antimony be put into a retort, and four parts of clear concentrated Oil of Vitriol poured on it, as soon as the Acid is heated it turns brown, and emits a most suffocating smell of Sulphur, which increases as the Regulus is penetrated and corroded by the Acid.

On raising the fire, there separates from it a matter that seems mucilaginous; and when the Acid hath boiled some time, the Regulus is converted into a white saline mass, as Mercury is in the preparation of Turbith mineral. At the same time a little Sulphur sublimes into the neck of the retort. At last all the Oil of Vitriol passes over into the receiver, and leaves the Regulus in a white, spungy, saline mass in the retort. When the fire is out, the vessels unluted, and the receiver separated from the retort, there rises a white vapour like that of the smoking liquor of Libavius.

The saline mass left in the retort, after the operation, is found increased to near double its weight: this increased weight is owing to the Acid that hath united with the Regulus.

This combination of the Vitriolic Acid with the Regulus of Antimony is excessively caustic, and cannot, for that reason, be administered internally.

The purest Spirit of Salt hath no sensible effect either on Antimony or its Regulus: but if Antimony be coarsely pounded, it separates therefrom, though slowly, some light, sulphureous flakes.

The action of Spirit of Nitre on this metallic substance is more perceptible: by little and little it attacks the plates of the Antimony, which discharge a great number of air-bubbles. As the dissolution advances, the Acid acquires a greenish colour inclining to blue; and if there be not too much of it, it will be almost entirely imbibed by the Antimony, penetrate between its laminæ, and exfoliate them in the direction of the needles that compose them. If there be too much of the Acid, that is, if it rise above the Antimony, it will destroy these plates, and reduce them to a white powder.

But when the Acid is imbibed slowly, we discover between the swelled laminæ little saline transparent crystals, that vegetate much in the same manner as those of the pyrites, in which small crystals of Vitriol are frequently observed, whose figures are not very well determined. These little crystals between the Antimonial plates are intermixed with yellow particles, which being carefully separated burn like common Sulphur.

All these useful observations, concerning the action of the Acids on Antimony and its Regulus, we owe likewise to Mr. Geoffroy; who advises the collecting a quantity of these little crystals in time; because they disappear soon after they are formed, being probably covered by the white powder, or magistery, which is continually produced as fast as the Nitrous Acid disunites and separates the needle-like fibres of the Antimony.

Mr. Geoffroy observed the same sort of crystals on the Regulus of Antimony, when substituted for crude Antimony in this experiment; but it requires a great deal of care to separate these crystals; for as soon as the air comes into contact with them they lose their transparency; and if you wait till the Regulus be in some measure converted into a magistery, they are not then to be distinguished.

In order therefore to have a good view of these crystals, the Regulus must be broken to pieces; these pieces put in a glass bason, and Spirit of Nitre poured on them to half their heighth, but not to cover them. This Acid penetrates them, exfoliates them in white scales; and on the surface of these scales the crystals shoot of a dead white colour. In two or three days time these crystals vegetate and grow in the form of cauli-flowers: they must then be gathered, to prevent their being confounded in the white magistery which continues to be produced, and would not suffer them to be distinguished. If you attempt to dissolve the reguline part of Antimony by an aqua regis compounded in different proportions, and applied in a different dose from what is prescribed in the process, the Regulus of Antimony will only be calcined, as it is by the other Acids, and will precipitate in the form of a white magistery as fast as it dissolves, so that no part thereof will remain united with the solvent. The proof of this is, that if an alkaline liquor be poured, even to the point of saturation, upon the aqua regis that hath thus dropt the Antimony, no new precipitate will be deposited.

PROCESS XI.

Regulus of Antimony combined with the Acid of Sea-salt. Butter of Antimony. Cinabar of Antimony.

Pulverize and mix thoroughly six parts of Regulus of Antimony, and sixteen parts of Corrosive Sublimate. Put this mixture into a glass retort that hath a wide short neck, and let one half of its body at least be left empty. Set it in a reverberatory furnace, and having fitted a recipient thereto, and luted the joint, make a very small fire at first, to heat it slowly. Increase it afterwards by degrees, till you see a liquor ascend from the retort that grows thick as it cools. Keep up the fire to this degree as long as you see any of this matter come over.

When no more rises with this degree of fire, unlute your vessels, take off the receiver, and in its place substitute another filled with water. Then increase your fire by degrees till the retort be red-hot. Some running Mercury will fall into the water, which you may dry and keep for use; it being very pure.

OBSERVATIONS.

In our observations on the preceding process, we took notice that the purest Marine Acid, in the form of a liquor, will not dissolve the reguline part of Antimony. Here this very Acid combined with Mercury, and applied in a dry form to the Regulus of Antimony, quits the Mercury with which it was united, in order to join this very Regulus, as having a greater affinity therewith. This operation is a further proof of what we advanced on the subject of Mercury; to wit, that several metallic substances, which are not soluble by certain Acids when in a fluid state, may be dissolved by those Acids when most highly concentrated; as they are when combined with any other substance in a dry form, and are separated from it by the force of fire. Their efficacy is also further promoted by their being reduced, on this occasion, into subtile vapours.

The Marine Acid combined with the reguline part of Antimony doth not form a hard, solid compound; but a kind of soft substance, that melts in a very gentle heat, and also becomes fixed by the least cold, much in the same manner as butter; and from this property it hath its name.

Soon after mixing the Regulus with the Corrosive Sublimate, the matter sometimes grows considerably hot: this is occasioned by the Marine Acid's beginning to act on the reguline part, and to desert its Mercury.

The Butter of Antimony rises with a very moderate heat; because the Acid of Sea salt hath the property of volatilizing, and carrying up along with it, the metallic substances with which it is combined: and for this reason a very gentle heat only is required at the beginning of the operation.

It is absolutely necessary that the neck of the retort be wide and short: for otherwise if the Butter of Antimony should fix and be accumulated therein, it might stop up the passage entirely, and occasion the bursting of the vessels. By this operation we obtain eight parts and three quarters of fine Butter of Antimony, and ten parts of running Mercury; there being left in the retort one part and a half of a rarefied matter, black, white, and red. This is probably the most earthy and most impure part of the Regulus of Antimony.

It is of the utmost consequence to the operator that he avoid with the greatest care the vapours that issue from the vessels, because they are extremely noxious, and may occasion mortal disorders. The Butter of Antimony is a most violent Corrosive and Caustic.

When all the Butter is risen, the receiver is shifted in order to receive the Mercury; which, being disengaged from the Acid that gave it a saline form, appears in its natural form of Quick-silver: but it requires a much greater degree of heat than the Butter of Antimony to raise it by distillation.

If crude Antimony, instead of Regulus of Antimony, be mixed with Corrosive Sublimate, a Butter of Antimony will be obtained in the same manner; but, instead of having a running Mercury after the Butter, you will find a Cinabar sublimed into the neck and upper concavity of the retort.

The reason of this difference is easily conceived: for when the Regulus is used, the Mercury being deserted by its Acid finds no other substance to unite with, and so rises in the form of Quick-silver; but when crude Antimony is employed instead of its Regulus, as the reguline part thereof cannot combine with the Acid without quitting its Sulphur, so this Sulphur, being at liberty, unites with the Mercury, which is so likewise, and therewith forms a Cinabar; which from its origin is named Cinabar of Antimony. When you intend to make both Butter and Cinabar of Antimony at the same time, six parts of Antimony must be mixed with eight of Corrosive Sublimate; and care must be taken, while the Butter is coming over, to warm the neck of the retort by holding some live coals near it, with the precautions necessary to avoid breaking it. This warmth makes the Butter melt and run into the receiver; whereas, being thicker and of a much denser consistence than that made with the Regulus, it would otherwise gather in the neck of the retort, choak it entirely, and burst the vessel.

When the Butter is drawn from crude Antimony, more circumspection is necessary to make it of a beautiful white colour, than when it is obtained from the Regulus: for, if the fire be too strong during the distillation, or if the receiver be not soon enough separated from the neck of the retort, certain red sulphureous vapours, the fore-runners of the Cinabar, will at last ascend, and mixing with the Butter give it a brown colour.

In order to restore its beauty it must be put into a clean retort, and rectified by distilling it over again with a gentle sand-heat. By this rectification the Butter of Antimony becomes more fluid; and by re-distilling it a second time you may give it the thinness and fluidity of an oil.

After the operation there will be found in the receiver three parts and three quarters of Butter of Antimony, and some small crystals adhering to its inside, in the form of sprigs. When you break the retort there exhales from it a sulphureous odour; and you will find in it seven parts of Cinabar of Antimony, the greatest part of which is usually in compact glebes, that are heavy, smooth, shining, blackish throughout most of the mass, but in some places red: another part thereof appears in shining needles, and the rest in powder.

When all the Butter of Antimony is come over, and you begin to see the red vapours that predict the approaching ascent of the Cinabar, the receiver containing the Butter must be removed, lest the colour of the Butter should be spoiled by those sulphureous vapours. Another receiver is usually fitted on, without luting; in which a small quantity of running Mercury is sometimes found, when the operation is finished.

There remains, at the bottom of the retort, a fixed, shining, crystalline, black mass, which may be reduced to a Regulus by the common method.

Butter of Antimony may also be obtained from a mixture of Antimony with any of the other preparations of Mercury in which the Acid of Sea-salt is an ingredient; such as sweet Sublimate, the Mercurial Panacea, and White Precipitate: but as none of these combinations contain so great a proportion of that Acid as is in the Corrosive Sublimate, the Butter obtained by their means is far from being so caustic and so fiery as that which rises from a mixture of Antimony, or its Regulus, with Corrosive Sublimate.

Silver precipitated by the Acid of Sea-salt, and ready to be melted into a Luna cornea, being mixed with powdered Regulus of Antimony yields likewise a Butter of Antimony.

If you propose to make it by this means, you must mingle one part of the Regulus of Antimony in powder with two parts of the Precipitate; put this mixture into a glass retort of such a size that it may fill but one half thereof; set it in a furnace; apply a receiver; begin with a gentle heat, which will make a clear liquor come over; and then increase your fire by degrees. White vapours will rise and condense into a liquid Butter; and in the mean time there will be a slight ebullition in the receiver, attended with a little heat. Continue the fire till nothing more will come over; then let your vessels cool and unlute them.

You will find in the receiver an Oil or Butter of Antimony, partly fluid and partly congealed, somewhat inclined to yellow, weighing an eighth part more than the Regulus of Antimony made use of.

The inside of the retort will be carpeted over with small white flowers, of a brilliant silver colour, and an acid taste; and in the bottom of the retort will be found a hard, compact, ponderous mass, difficult to break, yet falling of itself to a powder; its colour externally grey, white, and blueish; internally black, and shining much like Regulus of Antimony; having a saltish taste on its surface, and weighing about a sixteenth less than the Precipitate of Silver employed in the operation.

This experiment demonstrates that the Acid of Sea-salt hath a greater affinity with Regulus of Antimony than with Silver.

The Butter of Antimony prepared by this method is somewhat less caustic than that made with Corrosive Sublimate. It is called the Lunar Butter of Antimony.

The effervescence that arises in the receiver is remarkable. Probably the Acid of Sea-salt, though reduced into vapours when it ascends out of the retort, is not yet perfectly combined with the reguline part of the Antimony, which it nevertheless carries over with it, and the union is completed in the receiver; which occasions the effervescence observed.

The little white silvery flowers, adhering to the inside of the retort, are flowers of Regulus of Antimony, which sublime towards the end of the distillation.

The compact mass, found at the bottom of the retort, is no other than the Silver separated from its Acid, and combined with a portion of the Regulus of Antimony. The colours and the saltish taste of its surface are occasioned by a remainder of the Marine Acid. This Silver is rendered brittle and eager by the union it hath contracted with some of the Regulus of Antimony.

It is easy to purify it, and restore its ductility, by separating it from the Regulus of Antimony. There are several ways of doing this: one of the most expeditious is to flux it with Nitre, which burns and converts to a calx the semi-metal with which the Silver is adulterated.

PROCESS XII.

Butter of Antimony decompounded by means of Water only. The Pulvis Algaroth, or Mercurius Vitæ. The Philosophic Spirit of Vitriol.

Melt with a gentle heat as much Butter of Antimony as you please. When it is melted, pour it into a large quantity of warm water. The water will immediately grow turbid, but whitish, and let fall a great quantity of white powder. When all the precipitate is settled, decant the water: pour on fresh warm water; and having thus edulcorated it by several ablutions, dry it, and you have the Pulvis Algaroth, or Mercurius Vitæ.

OBSERVATIONS.

In the preceding processes we observed that the Marine Acid will not dissolve the reguline part of Antimony, unless it be very highly concentrated, and more so than it can possibly be while in the form of a liquor. Of this the experiment before us is a further proof. Whilst the Marine Acid is so perfectly dephlegmated, as it is in Corrosive Sublimate and Butter of Antimony, it remains combined with the reguline part of Antimony; but if this combination be dissolved in water, the moment the Acid is weakened by the interposition of the particles of water, it becomes incapable of continuing united with the semi-metal which it had before dissolved; deserts it, and lets it fall in the form of a white powder.

The Pulvis Algaroth is therefore no other than the reguline part of Antimony, attenuated and divided by the union it had contracted with the Acid of Sea-salt, and afterwards separated from that Acid by the intervention of water alone. The proof is, that this powder retains none of the properties of the Butter of Antimony: it is neither so fusible nor so volatile; on the contrary, it is capable of sustaining a very strong degree of fire, without subliming and without melting: it may be reduced to a Regulus: it hath not now the same caustic nature: it is only an emetic; which however is extremely violent, and on that account is never prescribed by any prudent physician.

Another proof, that the Marine Acid is separated from the Regulus of Antimony in the precipitation of the Pulvis Algaroth, is, that the water in which this precipitation is made becomes acid, or a sort of weak Spirit of Salt. If it be evaporated, and concentrated by distillation, a very strong acid liquor may be obtained from it. This Acid goes, very improperly, by the name of the Philosophic Spirit of Vitriol; for it is rather a Spirit of Salt.

The Pulvis Algaroth, made with Butter of Antimony procured from the Regulus, is whiter than that made with Butter of Antimony procured from crude Antimony; probably because the latter always retains some sulphureous particles.

Butter of Antimony exposed to the air attracts the moisture thereof, and partly runs into a liquor; but, as fast as this liquor is produced, it deposites a white sediment, which is an actual Pulvis Algaroth. This also is very agreeable to what we advanced touching the decomposition of Butter of Antimony by the addition of water. The Butter attracts the moisture of the air, because the Acid it contains is exceedingly concentrated; and this moisture produces the same effect as water purposely added.

PROCESS XIII.

Bezoar Mineral. The Bezoartic Spirit of Nitre.

Melt Butter of Antimony over warm ashes, and put it into a phial or matrass. Gradually pour on it good Spirit of Nitre, till the matter be entirely dissolved. This usually requires as much Spirit of Nitre as there is Butter of Antimony. During the dissolution fumes will rise, which must be carefully avoided. Pour your solution, which will be clear and of a reddish colour, into a glass cucurbit, or a pan of stone-ware: set it in a sand-bath, and evaporate to dryness with a moderate heat. There will be left a white mass, weighing a fourth part less than the whole quantity used, both of the Butter and the Spirit of Nitre. Let it cool, and again pour on it as much Spirit of Nitre as you used the first time. Place the vessel again in the sand-bath, and evaporate the moisture as before. You will have a white mass that hath neither gained nor lost in weight. On this pour, for the third time, the same quantity of Spirit of Nitre as you did the first time. Again evaporate the moisture to perfect dryness: then increase your fire, and calcine the matter for half an hour. You will have a dry, friable, light, white matter, of an agreeable acid taste; which will fall into a coarse powder, and must be kept in a phial carefully stopt. This is Bezoar Mineral: it is neither caustic nor emetic, and has only a sudorific virtue. It obtained the name it bears, because, like the animal Bezoar, it was imagined to have the property of resisting poison.

OBSERVATIONS.

It is not surprising that the Nitrous Acid poured on Butter of Antimony should dissolve it, and unite with it: for with the Marine Acid, which makes a part of this combination, it forms an aqua regis, which we know is the true solvent of the reguline part of Antimony. But in this dissolution, and the changes it produces, there are some things very remarkable and worthy of attention. 1. The Nitrous Acid, by uniting with the Butter of Antimony, deprives it of its property of rising with a very gentle heat, and makes it much more fixed: it can now be dried, and suffer all its moisture to be evaporated; which is not to be done with pure Butter of Antimony: for that, being exposed to a certain degree of heat, instead of letting go its moisture and remaining dry, rises wholly, without the least appearance of any separation of parts.

2. The Butter of Antimony, which, before its combination with the Nitrous Acid, is a most violent Caustic and Corrosive, becomes so mild after it, that it may not only be taken internally without danger, but hath scarce any sensible operation.

The following considerations will lead us to a reasonable explanation of these phenomena. 1. The Nitrous Acid, when combined with metallic substances, doth not communicate to them the same volatility as they acquire from the Marine Acid. Hence it follows, that, if the Nitrous Acid be added to any combination of a metallic substance with the Marine Acid, this new compound will be rendered less volatile, and consequently more able, without rising in vapours, to bear a degree of heat sufficient to carry off part of its Acid. This is the case with Butter of Antimony, after Spirit of Nitre is mixed with it; especially considering, 2. That the Nitrous Acid cannot unite with the reguline part of the Butter of Antimony without weakening the connection between it and the Marine Acid; whence it follows, that the combination of the Nitrous Acid further facilitates the separation of the Marine Acid from the Regulus. Now as soon as the Marine Acid quits the reguline part, that part becomes more fixed, and consequently more capable of enduring the degree of heat requisite to discharge all the adhering Acid; and not only the Marine, but even the Nitrous also. It is not therefore surprizing that, after the Antimony which remains combined with the Nitrous Acid is dried, it should not possess that corrosive power which it derives only from the Acids wherewith it is armed. In order to free it more perfectly from all Acid, we order the fire to be increased after the third desiccation; and the remainder of the Butter of Antimony to be calcined for a full half-hour longer.

That the Marine Acid is separated from the reguline part of the Butter of Antimony, by the desiccations it undergoes in converting it into Bezoar, is proved by this, that, when these desiccations are performed in close vessels, the liquor drawn off is a true aqua regis, known by the name of the Bezoartic Spirit of Nitre.

It remains to be considered why the Bezoar mineral, though freed from all acid, is not emetic; while the Pulvis Algaroth, which is likewise the reguline part of the Butter of Antimony deprived of its Acid, is such a violent emetic, and even to be dreaded for its remaining causticity.

In order to discover the reason of this difference, it is proper to observe that, when we say Bezoar mineral and the Pulvis Algaroth contain no Acid, we must not be understood in too strict a sense: on the contrary, there is reason to think that a certain quantity of Acid still remains in each of them; which however is scarce worth notice, in comparison of the quantity each contained at first. This being allowed, it will not be hard to find the difference between these two preparations of Antimony. The Pulvis Algaroth is deprived of its Acid by the addition of water alone, which only carries off all the loose Acid it can take up, without making any change in the nature of that which continues in combination with the reguline part. Now, as the Marine Acid is not intimately united with the reguline part in Butter of Antimony; as it still retains some of its properties, such as attracting the moisture of the air, giving manifest tokens of its Acid nature, &c.; and as the corrosive quality of this compound depends on this last in particular; the small portion of Acid left in the Pulvis Algaroth will in some degree preserve its former character: and hence comes the effect of this powder, which still retains a little of the corrosive quality that belonged to the Butter of Antimony.

But this is not the case with the small remainder of Acid, which possibly still continues united with the Bezoar mineral prepared as here directed. This compound hath been exposed to a fire sufficient, not only to dry it, but even to calcine it. Now fire is capable of producing great changes in the texture of bodies. It must have forced off from the Bezoar all the Acid that was not intimately combined with it; and that part which it could not drive off, because of its obstinate adhesion, it must have further united and combined more closely with the metallic earth: for we see that fire greatly promotes the action of solvents on the matters with which they are united.

With regard to the properly emetic quality of the Pulvis Algaroth, it cannot be imputed to the combination of any Acid with that powder; since we see that the most powerfully emetic preparations of Antimony, viz. its Regulus and Glass, contain no Acid: it must therefore be attributed to some cause different from that on which its corrosive quality depends. This cause we shall easily find by attending to the different manners in which the Marine Acid, when alone and in aqua regia, operates on the reguline part of Antimony.

The Marine Acid alone dissolves the Regulus of Antimony, but with great difficulty; nor doth it effect a complete dissolution thereof, as is evident from what hath been already said: whereas the Marine Acid, combined with the Nitrous Acid, and therewith forming an aqua regis, as in the preparation of Bezoar, dissolves the reguline part of Antimony completely and radically. Now, it is certain that, the more efficaciously Acids operate on metallic substances, the more of their phlogiston do they destroy; and we cannot but recollect that the preparations of Antimony are so much the less emetic the less phlogiston they contain, or the further they recede from the nature of a Regulus, and the nearer they approach to that of Diaphoretic Antimony: consequently it is plain how Bezoar mineral, which is a sort of calx of Antimony entirely deprived of its phlogiston by the intimate dissolution thereof made by the Acids of the aqua regis, may be in no degree emetic; while the Pulvis Algaroth, being a true Regulus of Antimony, on which the Marine Acid hath operated but very superficially, and which still contains a great deal of phlogiston, is a most violent emetic.

PROCESS XIV.

Flowers of Antimony.

Take an unglazed earthen pot, having an aperture in its side, with a stopple to shut it close. Set this pot in a furnace, the cavity whereof it may fit as exactly as possible; and fill up with lute the space, if any, left between the vessel and the furnace. Over this vessel fix three aludels, with a blind-head at the top; and light a fire in the furnace under the pot.

When the bottom of the pot is thoroughly red, throw into the lateral aperture a small spoonful of powdered Antimony. Stir the matter immediately with an iron spatula made a little bending, in order to spread it over the bottom of the vessel, and then stop the hole. The flowers will rise and adhere to the insides of the aludels. Keep up the fire so that the bottom of the pot may always continue red; and, when nothing more sublimes, put in a like quantity of Antimony, and operate as before. In this manner go on subliming your Antimony, till you have as many flowers as you want. Then let the fire go out; and when the vessels are cold unlute them. You will find flowers adhering all round the insides of the aludels and the head, which you may collect with a feather.

OBSERVATIONS.

Antimony is a volatile mineral, capable of being sublimed into flowers; but this cannot be effected without occasioning a notable change in its parts. The reguline and the sulphureous parts are not united so intimately, or in the same proportion, in the flowers as in the Antimony itself; and accordingly we find these flowers have a strong emetic quality, which Antimony hath not. They are of divers colours; which probably arises from their containing more or less Sulphur. Three or four aludels are placed one over another, not only with a view to provide a greater surface, to which the flowers may adhere, but also to give them room enough to circulate, without which they might burst the vessels.

If you introduce the nosle of a pair of bellows into the pot that contains the Antimony, and blow upon it, the sublimation of the flowers will be much sooner effected. This is a general rule with regard to all matters that are to be sublimed or evaporated; the reason of which we have already given.

It is proper that no interval be left between the furnace and the pot containing the Antimony, lest the heat should be thereby communicated to the aludels, on which the flowers fasten best when they are cold.

After the operation, there remains at the bottom of the pot a portion of Antimony half calcined; which being pulverized, and thoroughly calcined till it emit no fume, may be employed to make the Glass of Antimony.

PROCESS XV.

Regulus of Antimony converted into Flowers.

Pulverize your Regulus of Antimony: put the powder into an unglazed earthen pot: three or four fingers breadth above the powder, fit into the pot a little cover, made of the same earth, and having a small hole in its middle, so that it may with ease be placed in the pot, and taken out when there is occasion: cover the mouth of the pot with a common lid; set it in a furnace, and kindle a fire under it sufficient to make the bottom of the pot red, and to melt the Regulus. When it hath been thus kept in fusion for about an hour, let the fire go out, and the whole cool. Then remove the two covers. You will find adhering to the surface of the Regulus, which will be in a mass at the bottom of the pot, white flowers resembling snow, intermixed with beautiful, brilliant, silver-coloured needles. Take them out, and you will find them make about one part in sixty-two of the whole Regulus employed.

Put the covers again in their places, and proceed in the same manner as before; when the vessels are cold you will find half as many more flowers as you got the first time.

Proceed thus till you have converted all your Regulus into flowers. This will require a considerable number of sublimations, which, as you advance, will always yield you a greater portion of flowers; respect, however, being had to the quantity of Regulus remaining in the pot.

OBSERVATIONS.

We must here repeat what we said just before, in our observations on the preceding process; viz. that Regulus of Antimony is capable of being wholly elevated and sublimed by the action of fire; but that it must at the same time undergo a considerable change and alteration. These flowers of Regulus of Antimony are very different from every other Antimonial preparation. They resemble the Pearly Matter in this, that they cannot be reduced to a Regulus by any means whatever: but they differ from it, 1. in that they are not fixed; for, when melted by fire, they fly wholly away in vapours: 2. in that they are capable of being dissolved by aqua regis, much in the same manner as the Regulus; whereas the Pearly Matter is known to be indissoluble by any Acid.

As soon as Regulus of Antimony is in fusion, it begins to sublime into flowers; so that it is needless to apply a greater degree of heat than is just sufficient to melt it.

A pan of some width is preferable to a crucible for this operation; because the upper surface of the Regulus melted therein is larger, and, the larger that surface is, the more considerable is the quantity sublimed from it.

The two covers which are applied within and over the pot are designed to check, as much as possible, the dissipation of the melted Regulus; yet without absolutely excluding the free access of the air, the concourse of which is useful in all metallic sublimations. Notwithstanding these precautions, it is impossible to prevent the escape of some of the Regulus, in vapours that cannot be confined. Somewhat less than three fourths of the Regulus made use of is nearly the yield in flowers: the rest evaporates through the interstices left by the covers, which must not be luted for the reason just assigned.

CHAP. II.

Of BISMUTH.

PROCESS I.

To extract Bismuth from its Ore.

Break the ore of Bismuth into small pieces, and therewith fill a crucible either of earth or iron. Set the crucible in a furnace, and light such a fire that the bits of ore may become moderately red. Stir the ore from time to time, and, if you perceive it crackle and fly, keep the crucible covered. At the bottom you will find a button of Bismuth.

OBSERVATIONS.

The extraction of Bismuth from its ore requires nothing but simple fusion, without the addition of any inflammable matter, because it is naturally possessed of its metalline form. Nor does it require any flux; because it is very fusible: which allows us to melt it, and collect it in a mass, without the necessity of fusing likewise the earthy and stony matters in which it is lodged. These matters remain in their first state; and the melted Bismuth descends by its gravity to the bottom of the crucible. No greater degree of heat must be applied, on this occasion, than is necessary to melt the semi-metal: for, as it is volatile, part of it would be dissipated; so that much less thereof would be obtained, if the fire were made too strong, and so much the less as another portion thereof would be converted into a calx. For the same reason, the crucible must be taken out of the furnace as soon as you perceive that all the Bismuth contained in the ore is melted, and that the button doth not increase.

The ore of Bismuth may also be treated like the ores of Lead and Tin; that is, it may be reduced into a fine powder, mixed with the black flux, a little Borax, and Sea-salt; put into a close crucible, and fused in a melting furnace. In that case you will find a button of Regulus covered with scoria. By this method rather more Bismuth is obtained; and it is best to make use of it when the ore is poor, because, in such a case, none at all would be obtained by the other process. But here care must be taken to apply at once the degree of fire necessary to melt the mixture: for, if it remain long in the fire, much Bismuth will be lost, on account of the great volatility of this semi-metal, and the facility with which it turns to a calx.

Bismuth is pretty frequently found pure in its earthy and stony matrices; and when mineralized it is usually so by Arsenic, which, being still more volatile, flies off in vapours while the ore is melting, provided it be but in a small quantity: if there be much of it, and the ore be smelted by fusing it with the black flux, the Arsenic also is reduced to a Regulus, unites more intimately with the Bismuth, becomes a little more fixed by that union, and increases the quantity of the semi-metallic mass found after the fusion.

Though Bismuth be not usually mineralized by Sulphur, that is not because it is incapable of uniting therewith; for, if equal parts of Bismuth and Sulphur be melted together, after the fusion the Bismuth will be found increased near an eighth part, and formed into a mass disposed in needles much like Antimony.

When we come to treat of the ore of Arsenic, we shall have occasion to say a good deal more concerning Bismuth and its ore; because these minerals resemble each other very much.

Mr. Geoffroy, son of the Academician, hath shewn in a Memoir read before the Academy of Sciences, that there is a great resemblance between Bismuth and Lead. That Memoir, which contains only the beginning of Mr. Geoffroy's course of experiments, proves that the author supports with dignity the glory of his name. It is there demonstrated, by a very great number of experiments, that fire produces the same effects on Bismuth as on Lead. This semi-metal is converted into a calx, into litharge, and into glass, as Lead is; and these productions have the same properties as the preparations of Lead made with the same degree of fire. Bismuth is capable of vitrifying all the imperfect metals, and of carrying them off through the pores of the crucible. So that Gold and Silver may be purified and cupelled by its means, as well as with Lead. You may on this occasion turn to what we have said concerning Lead.

PROCESS II.

Bismuth dissolved by Acids. Magistery of Bismuth. Sympathetic Ink.

Into a matrass put Bismuth broken into little bits: pour on it, by little and little, twice as much aqua fortis. This Acid will attack the semi-metal briskly, and dissolve it entirely, with heat, effervescence, vapours, and puffing up. The solution will be clear and limpid.

OBSERVATIONS.

Of all Acids the Nitrous is that which best dissolves Bismuth. It is not necessary, on this occasion, to place the phial, in which the dissolution is performed, on a sand-heat, as in most other metallic dissolutions: on the contrary, care must be taken not to pour on all the aqua fortis at once; because it operates with so much activity that the mixture will heave up and run over the vessel.

The bare addition of water is sufficient to precipitate the solution of Bismuth. If this solution be mixed with a very large proportion of water, the liquor grows turbid, appears milky, and deposites a precipitate of a very beautiful white. This is that white which the ladies use at their toilets.

Water produces this precipitation by weakening the Acid; which probably is incapable of keeping the Bismuth dissolved, unless it have a certain degree of strength.

If you would have a Magistery of Bismuth beautifully white, you must perform the dissolution with an aqua fortis that is not tainted with any mixture of the Vitriolic Acid; for this gives the precipitate a dirty white colour, inclining to grey. Several authors advise the use of a solution of Sea-salt, instead of pure water, for precipitating the Bismuth, imagining that this Salt will effect a precipitation here as it does in the cases of Silver and Lead. But Mr. Pott, a German Chymist, who hath published a long dissertation on Bismuth, pretends, on the contrary, that neither Sea-salt, nor its Acid, is capable of precipitating this semi-metal; and that when a precipitation takes place on mixing them with our solution, it is brought about only by means of the water in which those substances are diffused.

Bismuth may also be precipitated by the means of Fixed or Volatile Alkalis; but the precipitate is not of so fine a white as when procured by the means of pure water only.

If a greater quantity of aqua fortis, than that prescribed in the process, be made use of to dissolve the Bismuth, a great deal more water will also be required to precipitate the Magistery; because there will be much more Acid to weaken. This white ought to be well washed, in order to free it from any remainder of acidity; and it should be kept in a bottle well stopped; because the access of the air makes it turn brown, and if any of the Acid be left it will turn it yellow.

A solution of Bismuth prepared with the proper quantity of aqua fortis, that is, with two parts of the Acid to one of the semi-metal, concretes into little crystals almost as soon as made.

Aqua fortis not only acts on Bismuth when separated from its ore, and reduced to a Regulus, but attacks it even in its ore, and likewise dissolves at the same time some portion of the ore itself. With this solution of the ore of Bismuth Mr. Hellot makes a very curious Sympathetic Ink, differing from all that were known before.

Mr. Hellot prepares the liquor in the following manner: "He bruises the ore of Bismuth to a coarse powder. On two ounces of this powder he pours a mixture of five ounces of common water with five ounces of aqua fortis. He does not heat the vessel till the first ebullitions are over. He then sets it in a gentle sand-heat, and lets it digest there till he sees no more air bubbles rise. When none appear in this heat, he increases it so as to make the solvent boil slightly for a full quarter of an hour. It takes up a tincture nearly of the colour of brown beer. The ore that gives the aqua fortis this colour is the best. He then lets the solution cool, laying the matrass on its side, that he may decant the liquor more conveniently when all is precipitated that is not taken up by the solvent.

"The second vessel, into which the liquor is first decanted, he also lays declining, that a new precipitation of the undissolved matters may be obtained; after which he pours the liquor into a third vessel. This liquor must not be filtered, if you would have the rest of the process succeed perfectly; because the aqua fortis would dissolve some of the paper, and that would spoil the colour of your paper.

"When this solution, which Mr. Hellot calls the Impregnation, is thoroughly clarified by being decanted three or four times, he puts it into a glass bason with two ounces of very pure Sea-salt. The fine white salt made by the sun succeeded best with Mr. Hellot. If that cannot be had, common bay-salt, purified by solution, filtration, and crystallization, may be used instead of it. But as it is rare to meet with any of the sort that is not a little tainted with iron, the white bay-salt is to be preferred. The glass bason he sets in a gentle sand-heat, and keeps it there till the mixture be reduced by evaporation to an almost dry saline mass.

"If you desire to save the aqua regis, the impregnation must be put into a retort, and distilled with the gentle heat of a sand-bath. But there is an inconveniency, as Mr. Hellot observes, in employing a retort; which is, that, as the saline mass cannot be stirred while it coagulates in the retort, it is reduced to a compact cake of coloured Salt, which presents but one single surface to the water in which it must be dissolved; so that the dissolution thereof takes up sometimes no less than five or six days. In the bason, on the contrary, the saline mass is easily brought to a granulated Salt, by stirring it with a glass rod; and, when thus granulated, it has a great deal more surface; it dissolves more easily, and yields its tincture to water in four hours time. Indeed one is more exposed to the vapours of the solvent, which would be dangerous, if the operation were to be often performed, without proper precautions.

"When the bason, or little vessel, containing the mixture of the Impregnation and Sea-salt is heated, the liquor, which was of an orange-coloured red, becomes a crimson red; and, when all the phlegm of the solvent is evaporated, it acquires a beautiful emerald colour. By degrees it thickens, and acquires the colour of a mass of Verdegris. It must then be carefully stirred with the glass rod, in order to granulate the Salt, which must not be kept over the fire till it be perfectly dry; because you run a risk of losing irrecoverably the colour you are seeking. You may be sure you have lost it, if by too much heat the Salt that was of a green colour become of a dirty yellow. If it be once brought to this state, it will continue without changing when cold: but if care be taken to remove it from the fire while it is still green, you will see it gradually grow pale, and become of a beautiful rose colour as it cools.

"Mr. Hellot removes it from this vessel, and throws it into another containing distilled rain water: and this second vessel he keeps in gentle digestion till he observes that the powder which falls to the bottom is perfectly white. If, after three or four hours digesting, this powder still continues tinged with a rose colour, it is a proof that water enough was not added to dissolve all the Salt impregnated with the tincture of the solution. In this case, the first tinged liquor must be poured off, and fresh water added, in proportion to the quantity of tinged Salt, that is supposed to remain mixed with the precipitate.

"When the ore is pure, and doth not contain a great deal of fusible stone, commonly called Fluor or Quartz, an ounce of it generally yields tincture enough for eight or nine ounces of water, and the liquor is of a beautiful colour like that of the lilach or pipe-tree blossom. In order to prove the effect of this tincture, you must write with this lilach-coloured liquor on good well-gummed paper, that does not sink: or you may use it to shade the leaves of some tree or plant, having first drawn the outlines thereof lightly, with China-ink or with a black-lead pencil. Let this coloured drawing, or writing, dry in a warm air. You will perceive no colour while it is cold; but if it be gently warmed before the fire, you will see the writing, or the drawing, gradually acquire a blue or greenish-blue colour, which is visible as long as the paper continues a little warm, and disappears entirely when it cools."

The singularity of this sympathetic ink consists in its property of disappearing entirely and becoming invisible, though it be not touched with any thing whatever: and this distinguishes it from all others; which, when once rendered visible by the application of proper means, do not again disappear, or at least not without touching the strokes on the paper with some other liquor.

Mr. Hellot made a vast variety of experiments on this subject, and gave his sympathetic ink successively the properties of all others that are known.

It follows from Mr. Hellot's experiments, that it is the Acid of Sea-salt which makes this saline magma of a green colour while it is hot: that without this Acid the saline matter continues red; and that the solution of Bismuth-ore in aqua fortis may therefore serve as a touchstone, to discover whether or no any unknown Salt under examination contains Sea-salt, or a portion of the Marine Acid.

He also proves, in the Memoirs he hath given in on this subject, that the Nitrous Acid is the true solvent of those ores of Bismuth which contain moreover Smalt and Arsenic. That Acid dissolves all the metallic and colouring matters contained in those ores, sparing nothing but the sulphureous and arsenical portion, the greatest part of which remains precipitated; and from this colouring matter the sympathetic ink derives its virtue.

Under the head of Arsenic we shall speak more amply of this matter in Cobalt, or the ore of Arsenic, that gives a blue colour to the sand with which it is vitrified.

The Vitriolic Acid does not, properly speaking, dissolve Bismuth. If to one part and an half of this semi-metal you add one part of Oil of Vitriol; distil the whole to dryness; and then lixiviate with water what remains in the retort; the liquor you obtained by this means will be of a reddish yellow colour, but will let nothing fall when mixed with an Alkali: and this shews that the Vitriolic Acid acts only upon the inflammable part of Bismuth, and doth not dissolve its metallic earth.

It dissolves the ore of Bismuth more perceptibly than Bismuth itself; because the ore contains, besides the reguline part, an arsenical matter, and a coloured matter, over which perhaps it hath more power.

The Acid of Sea-salt attacks and dissolves Bismuth in some small measure, but slowly and with difficulty. That this Acid dissolves a portion of our semi-metal may be proved, by mixing a Fixed or Volatile Alkali with Spirit of Salt in which Bismuth hath lain some time digesting; for then a precipitate falls.

But, though the Marine Acid be capable of dissolving Bismuth, it doth not follow that it hath a greater affinity than the Nitrous Acid with this metallic substance, as some Chymists have thought; who imagined that, in the precipitation of the Magistery of Bismuth by a solution of Sea-salt, the Acid of that Salt quits its basis to unite with the Bismuth which it precipitates, as is the case in the precipitations of Lead and of Silver by the same Salt, and that it forms, on this occasion, a Bismuthum corneum.

On this subject, Mr. Pott observed, 1. that, when only a small quantity of the solution of Sea-salt is mixed with the solution of Bismuth in the Nitrous Acid, no precipitate is formed: now it is certain that when the smallest quantity whatever of Sea-salt is mixed with the solution either of Lead or of Silver, a precipitate is immediately deposited, in a quantity proportioned to that of the Salt used.

2. Mr. Pott, having examined the precipitate of Bismuth thrown down by a solution of Sea-salt, found it not to have the properties of a metallic substance rendered horny: on the contrary, that precipitate being exposed to a very violent fire appeared refractory, and could not be melted.

CHAP. III.

Of ZINC.

PROCESS I.

To extract Zinc from its Ore, or Calamine.

Take eight parts of Calamine reduced to a powder; mix this powder accurately with one part of fine charcoal-dust, previously calcined in a crucible to free it from all moisture: put this mixture into a stone retort coated with lute, leaving a third part of it empty: set your retort in a reverberatory furnace, capable of giving a very fierce heat. To the retort apply a receiver, with a little water in it. Kindle the fire, and raise it by degrees till the heat be strong enough to melt Copper. With this degree of fire the Zinc being metallized will separate from the mixture, and sublime into the neck of the retort, in the form of metallic drops. Break the retort when it is cold, and collect the Zinc.

OBSERVATIONS.

The process here given for smelting Zinc out of Calamine is taken from the Memoirs of the Academy of Sciences at Berlin. The author of it is Mr. Marggraff, a skilful Chymist, whom we have already had occasion to mention under the article of Phosphorus.

Till this process was published, we knew no method of obtaining pure Zinc directly from the Lapis Calaminaris.

Most of the Zinc we have comes from an ore of difficult fusion that is worked at Goslar, and yields, at one and the same time, Lead, Zinc, and another metallic matter called Cadmia Fornacum, which also contains much Zinc, as we shall afterwards see.

The furnace used for smelting this ore is closed on its fore-side with thin plates or tables of stone, not above an inch thick. This stone is greyish, and bears a violent fire.

In this furnace the ore is melted amidst charcoal, by the help of bellows. Each melting takes twelve hours, during which time the Zinc flowing with the Lead is resolved into flowers and vapours, great part of which adheres to the sides of the furnace in the form of a very hard crust of earth. The workmen take care to remove this crust from time to time; for it would otherwise grow so thick at last as to lessen the cavity of the furnace very considerably.

There adheres moreover to the fore-part of the furnace, which is formed, as we said before, of thin plates of stone, a metallic matter, which is the Zinc, and is carefully collected at the end of each melting, by removing from this part all the live coals. A quantity of small coal is laid unlighted at the bottom; and on this small coal, by striking the stone plates gently with a hammer, the Zinc is made to fall out of the other matter, known by the Latin name of Cadmia Fornacum, among which it appears fixed in a radiated form. To this other matter we may properly enough give the name of Furnace-Calamine. The Zinc falls in the form of a melted metal, all on fire, and in a bright flame. It would soon be entirely burnt and reduced to flowers, as we shall see, if it were not extinguished, and easily cooled and fixed, by being hid under the unlighted small-coal placed below on purpose to receive it.

The Zinc adheres to the fore-part of the furnace preferably to any other, because that being the thinnest is therefore the coolest: and, in order further to promote its fixing on this part, they take care to keep the thin stone plates cool during the operation, by throwing water on them.

Hence it appears, that Zinc is not extracted from its ore by fusion and the precipitation of a Regulus, like other metallic substances. This is owing to the great volatility of our semi-metal, which cannot, without subliming, bear the degree of fire necessary to melt its ore. It is at the same time so combustible, that a great part of it rises in flowers which have not the metalline form.

Mr. Marggraff provides against these inconveniences by working the ore of Zinc in close vessels. By this means he prevents the Zinc from taking fire, and being converted into flowers; so that it sublimes in its metalline form. The water in the recipient serves to receive and cool the drops of Zinc that may be forced quite over the helm. As the operation requires a most violent fire, these drops must needs issue exceeding hot, and, without this precaution, break the recipient.

Mr. Marggraff by the same process extracted Zinc out of the Furnace-Calamine procured from ores containing Zinc; from Tutty, which is a sort of furnace-calamine; from the flowers and from the calx of Zinc; and from the precipitate of White Vitriol; all of them matters known to be Zinc, that wanted nothing but the phlogiston to give it a semi-metalline form, and from which nevertheless no body could ever before him procure any Zinc.

Mr. Marggraff observes, that the Zinc obtained by his process bears being flatted under the hammer into pretty thin plates; which the common Zinc will not do. The cause of this probably is, that the Zinc obtained by his method is more intimately combined with the phlogiston, and contains a greater quantity thereof, than that which is procured in the ordinary way.

PROCESS II.

To sublime Zinc into Flowers.

Take a very deep, large crucible: place it in a furnace, so that it may stand inclining in an angle of forty-five degrees nearly. Throw some Zinc into it, and kindle a fire in the furnace somewhat stronger than would be necessary to keep Lead in fusion. The Zinc will melt. Stir it with an iron wire, and there will appear on its surface a very bright white flame: two inches above this flame a thick smoke will be formed, and with this smoke exceeding white Flowers will rise, and remain some time adhering to the sides of the crucible, in the form of a very fine light down. When the flame slackens, stir your melted matter again with the iron wire: you will see the flame renewed, and the flowers begin again to appear in greater abundance. Go on thus till you observe that the matter will not flame, nor any more Flowers rise.

OBSERVATIONS.

Zinc takes fire very easily as soon as it is affected by a certain degree of heat; which proves, that in the composition of this semi-metal there is very much phlogiston, united but slightly with its metallic earth. The Flowers into which Zinc resolves, during its combustion, are of a perfectly singular nature, and differ greatly from all the other productions obtainable out of metallic substances.

They may be considered as the very calx of Zinc, or its metallic earth robbed of its phlogiston, and sublimed during the combustion of this semi-metal, being probably carried up by the phlogiston in flying off. For these Flowers, when once sublimed, are afterwards exceedingly fixed: they sustain the greatest violence of fire without rising, and are converted by it into a sort of glass.

None of the methods hitherto employed, for restoring to the Flowers of Zinc their metalline form, have ever succeeded. When treated like other metalline calces in a crucible, with every kind of inflammable matter, and different sorts of reducing fluxes, they never can be re-metallized: they only melt with the flux, and produce a kind of Glass.

Mr. Marggraff indeed, as mentioned before, obtained Zinc from these Flowers, by treating them as he did Calamine in a retort with charcoal-dust: but as the Flowers often carry up with them little particles of undecomposed Zinc, there still remains some doubt concerning the reduction of these Flowers, even by this method.

If the crucible, into which you put the Zinc to be converted into Flowers, instead of being left open, as directed, be covered with another crucible inverted, the two vessels luted together, placed in a melting furnace, and a strong fire immediately kindled and kept up for about half an hour; you will find, when the vessels are cold, that all the Zinc hath left the lower crucible, and is sublimed into the upper one, in its metalline form, without suffering any decomposition. This experiment proves, that Zinc, to be converted into Flowers, must necessarily be set on fire and burnt. As it cannot burn in close vessels, any more than other combustible bodies, and as it is volatile, it sublimes without suffering any decomposition. Regulus of Antimony and Bismuth may be sublimed in the same manner; but not so easily as Zinc, which is still more volatile than those other semi-metals.

It is necessary to stir the Zinc in fusion from time to time with an iron wire, when you intend to convert it into Flowers: for there forms on its surface a grey crust that obstructs its deflagration, and beneath which it is gradually converted into a clotted calx. In order, therefore, to promote the rising of the flowers, care must be taken to break this crust, as oft as it begins to form. On this there immediately appears a very bright white flame: two inches above the flame is seen a thick smoke, and with this smoke very white Flowers rise, that continue some time adhering to the inside of the crucible, in the form of a fine down.

M. Malouin, who, in sundry Memoirs on Zinc, hath endeavoured to discover what resemblance there is between this semi-metal and Tin, tried to calcine Zinc in the same manner as Tin; but found it somewhat more difficult. Zinc, while it is not in fusion, doth not calcine; but it begins to turn to a calx the moment it begins to melt. M. Malouin, having repeated the fusion of Zinc a great number of times, by that means collected at last a quantity of the calx of this semi-metal, resembling other metalline calces. This calx of Zinc he melted in a crucible with animal fat; whereby the calx was re-metallized, and reduced to Zinc. There is great reason to believe that the calx of Zinc made by this method is not so much burnt as the Flowers, and that it still contains a portion of phlogiston.

PROCESS III.

To combine Zinc with Copper. Brass. Prince's Metal, &c.

Pound one part and an half of Calamine, and an equal quantity of charcoal: mingle these two powders together, and moisten them with a little water. Put this mixture into a large crucible, or some other earthen vessel that will bear a melting heat. Amongst and over this mixture put one part of very pure Copper in thin plates, and then put fresh charcoal-dust over all: cover the crucible; set it in a melting furnace; put coals all round it, and let them kindle gradually. Raise the fire so as to make the crucible very red-hot. When you observe that the flame hath acquired a purple or bluish-green colour, uncover the crucible, and dip into it an iron wire, to examine whether or no the copper be in fusion under the charcoal-dust. If you find it is, moderate the force of the fire a little, and let your crucible remain in the furnace for a few minutes. Then take it out and let it cool: you will find your Copper of a gold colour, increased in weight a fourth, or perhaps a third part, and yet very malleable.

OBSERVATIONS.

The Lapis Calaminaris is not the only substance with which Copper may be converted into brass: all other ores containing Zinc, the Furnace-Calamine that sublimes where such ores are worked, Tutty, Zinc in substance, may be substituted for it, and, like it, will make very fine Brass; but, in order to succeed, sundry precautions are necessary which we shall now lay before you.

This process is a sort of cementation: for the Calamine doth not melt; only the Zinc is converted into vapours, and then combines with the Copper. On this the success of the operation partly depends, as it is the means of the Copper's preserving its purity and malleability; because the other metallic substances that may be united with the ore of Zinc, or with the Zinc itself, not having the same volatility, cannot be reduced to vapours. If you are apprised that the Calamine, or other ore of Zinc used on this occasion, is contaminated with a mixture of any other metallic matter, you must mingle luting earth with the charcoal-dust and the matter containing the Zinc; make it into stiff paste with water; of this make a bed at the bottom of your crucible, and ram it hard down; lay the Copper plates thereon, cover them with charcoal-dust, and then proceed as before. By this means when the Copper melts it cannot fall to the bottom of the crucible, nor mix with the ore; but is borne up by the mixture, and cannot combine with any thing but the Zinc, that rises in vapours, and, passing through the lute, fixes in the Copper.

Lapis Calaminaris, or other ore of Zinc, may also be purified before it be used for making Brass; especially if adulterated with Lead ore, which is often the case. For this purpose the ore must be roasted in a fire strong enough to give a small degree of fusion to the leaden matter; which will thereby be reduced into larger, heavier, and tougher masses. The most subtile particles are dissipated in the torrefaction, together with some of the Calamine. The Calamine, on the contrary, is by roasting made more tender, lighter, and much more friable. When it is in this condition, put it into a washing tray or van; dip the tray in a vessel full of water, and bruise the matter it contains. The water will carry off the lightest powder, which is the Calamine, and leave nothing at the bottom of the tray but the heaviest substance; that is the leaden matter, which is to be rejected as useless. The powder of the Calamine will settle at the bottom of the vessel, where, after pouring off the water, it may be found, and used as above directed.

In this operation the charcoal-dust serves to prevent both the Copper and the Zinc from being calcined: and for this reason, when you work on a great quantity of materials at once, it is not necessary to use so much charcoal-dust, in proportion, as when you work but on a small quantity; because, the greater the mass of metal, the less easily will it calcine.

Though the Copper melts in this operation, yet it is far from being necessary to apply such a strong fire as Copper usually requires to melt it: for the accession of the Zinc, on this occasion, communicates to it a great deal of fusibility. The increase of its weight is also owing to the quantity of Zinc combined with it. Copper acquires still another advantage by its association with this semi-metal; for it remains longer in the fire without calcining.

Brass well prepared ought to be malleable when cold. But in whatever manner it be made, and whatever proportion of Zinc there be in it, it is constantly found quite unmalleable when red-hot.

Brass melted in a crucible, with a fierce heat, takes fire almost like Zinc, and from its surface many white flowers ascend, dancing about in flakes like the flowers of Zinc. They are indeed the flowers of Zinc, and the flame of Brass urged by a strong fire is no other than the flame of the Zinc that is united with the Copper, and at that time burns. If Brass be thus kept long in fusion it will lose almost all the Zinc it contains. It will also lose much of its weight, and its colour will be nearly that of Copper. It is therefore necessary, towards performing this operation aright, to seize the moment when the Copper is sufficiently impregnated with Zinc, when it hath acquired the most weight and the finest colour, with the least detriment to its ductility, that is possible, and that instant to put out the fire; because, if the Copper be left longer in fusion, it will only lose the Zinc already united with it. Skill acquired by much practice, and an acquaintance with the particular Calamine employed, are necessary to guide the artist surely through this operation; for there are very considerable differences between the sundry ores of Zinc. Some of them contain Lead, as was said above, and in others there is Iron. When these heterogeneous metals come to be mixed with the Copper, they do indeed augment its weight, but they render it at the same time pale, and make it very harsh. Some Calamines require to be roasted before they can be used for this purpose, and in the torrefaction emit vapours of a Volatile Alkali, succeeded by vapours of a Sulphureous Spirit: others exhale no vapours while roasting, and may be employed without any antecedent preparation. These different qualities must evidently produce great differences in the operation.

Brass may also be made as Prince's metal and other imitations of Gold are actually made, by using Zinc in substance, instead of the ores that contain it. But these compositions have not, when cold, the ductility of Brass prepared with Lapis Calaminaris, because Zinc is seldom pure, or free from a mixture of Lead. Perhaps also the different manner in which the Zinc unites with the Copper may contribute to this variation.

To obviate this inconvenience, the Zinc must be refined from all alloy of Lead. The property of being indissoluble by Sulphur, which this semi-metal possesses, points out a very practicable method of doing it. The Zinc must be melted in a crucible, and stirred briskly with a strong iron wire, while tallow and mineral Sulphur are alternately projected upon it; but so that the quantity of Sulphur may greatly exceed that of the tallow. If the Sulphur do not burn entirely away, but form a kind of scoria on the surface of the Zinc, it is a sign that your semi-metal contains Lead. In this case you must continue throwing in more Sulphur, and keep stirring the Zinc incessantly, till you perceive that the Sulphur ceases to unite any more with a metallic substance, but burns freely on the surface of the Zinc. The semi-metal is then refined, because the Sulphur, which cannot dissolve it, unites very readily with the Lead, or other metallic substance, contained in it.

If Zinc thus refined be mixed with pure Copper, in the proportion of a fourth or a third part, and the mixture be kept in fusion and constantly stirring for some time, the Brass produced will be as ductile, when cold, as that made by cementation with the Lapis Calaminaris.

With regard to Prince's metal, and other imitations of Gold, they are made either with Copper or Brass re-combined with more Zinc. As it is necessary, for giving them a fine golden colour, to mix with them other proportions of Zinc than that acquired to make Brass only, they are generally much less ductile. In 1725, M. Geoffroy gave a Memoir on this subject in which he examined the effects of incorporating both Copper and Brass with Zinc, from a small to a very large quantity.

PROCESS IV.

Zinc dissolved in the Mineral Acids.

Weaken concentrated Oil of Vitriol by mixing with it an equal quantity of water. Into a matrass put the Zinc you intend to dissolve, first broken to small pieces. Pour on it six times its weight of the Vitriolic Acid, lowered as above directed, and set the matrass in a sand-bath gently heated. The Zinc will dissolve entirely, without any sediment. The Neutral Metallic Salt resulting from this dissolution shoots into crystals, which go by the name of White Vitriol, or Vitriol of Zinc.

OBSERVATIONS.

Though Zinc be soluble in all the Acids, and when combined with those Acids exhibits some uncommon phenomena, yet M. Hellot is the first that ever gave a particular account of what happens in those dissolutions: so that all we have to say on this head is extracted from that Gentleman's Memoirs. If a solution of Zinc in the Vitriolic Acid, prepared according to the directions in the process, be distilled from a retort placed in a sand-bath with a graduated heat, almost half the liquor presently comes over in pure phlegm. A small quantity of a Sulphureous Acid Spirit rises next. A greater force of fire is now requisite: the retort must therefore be removed into a reverberatory, and the distillation continued with a naked fire. On the first impression of this heat an odour of Liver of Sulphur discovers itself, which becomes sharp and suffocating towards the end of the distillation. In two hours time white vapours begin to appear, as in the rectification of common Oil of Vitriol. If the receiver be then shifted, you will obtain an Oil of Vitriol, in quantity about the eighteenth part of the whole used in the distillation, which, though sulphureous, is yet so concentrated, that, if a few drops thereof be poured into a weak Oil of Vitriol, they fall to the bottom with as much noise as if they were so many bits of red-hot iron, and heat this Oil of Vitriol as much as common Oil of Vitriol heats water.

At the bottom of the retort there remains a dry, white, crystalline, saline mass, exceeding in weight the Zinc that was dissolved, about a twelfth part of the whole weight of the liquor. The increase of its weight is owing to a portion of the Vitriolic Acid that remains concentrated in the Zinc, and could not be expelled by the fire. This portion of Acid adheres to it most tenaciously: for, though M. Hellot kept the retort containing it during two whole hours in so violent a fire that the vessel began to melt, the smallest vapour did not rise from it.

This saline caput mortuum is in the form of needles, much like the Sedative Salt. It is caustic, grows considerably hot when water is poured on it, and gives in the air, but slowly. Spirit of wine, digested with this Salt for eight or ten days, acquires the same smell as that which is mixed with concentrated Oil of Vitriol in preparing Æther.

Zinc is dissolved by the Nitrous and Marine Acids, much in the same manner as by the Vitriolic; except that the Marine Acid does not touch a black, spungy, rarefied matter, which it separates from the Zinc. M. Hellot found upon trial that this matter is not Mercury, and that it cannot be reduced to a metallic substance.

That ingenious Chymist distilled likewise Solutions of Zinc in the Nitrous and Marine Acids. There came over at first, as there did from the solution made by the Vitriolic Acid, an aqueous, and then an acidulated liquor. At last, by exciting the fire with great violence, towards the end of the distillation, he obtained a small quantity of the Acid that hath been employed in the dissolution: but the small portion of Acid thus obtained was exceeding strong; and the quantity of the Nitrous much more considerable than that of the Marine Acid.

A solution of Zinc in the Marine Acid, being distilled to dryness, yields a Sublimate on applying a violent heat to it.

All the Acids dissolve with ease, not only Zinc, but its Flowers also; and that nearly in the same quantity, and with almost all the same phenomena. M. Hellot, observing that the residues of most of the solutions of Zinc have a great resemblance with its flowers, is of opinion that this semi-metal may be reduced, by the means of solvents, to the same state into which it is brought by the fire when sublimed in Flowers.

CHAP. IV.

Of ARSENIC.

PROCESS I.

To extract Arsenic from its Matrices. Zaffre or Smalt.

Powder some Cobalt, white Pyrites, or other Arsenical matters. Put this powder into a retort with a short wide neck, leaving a full third thereof empty. Set your retort in a reverberating furnace; lute on a receiver; heat your vessel by degrees, and increase the fire till you see a powder sublime into the neck of the retort. Keep up the fire in this degree as long as the sublimation continues: when this begins to slacken, raise your fire, and make it as strong as the vessels will bear. When nothing more ascends, let it go out. On unluting the vessels, you will find in the receiver a little Arsenic in the form of a fine light farina. The neck of the retort will be full of white flowers, not quite so fine, some of which will appear like little crystals; and if a good deal of Arsenic be sublimed, a ponderous matter, like a white, semi-transparent glass, will be found adhering to that part of the neck of the retort which is next its body.

OBSERVATIONS.

Arsenic is a metallic substance still more volatile than Zinc; so that it cannot be separated from the matters with which it is mixed otherwise than by sublimation. It is proper, however, to take notice, that it is not naturally in a metallic form, and that, properly speaking, the whole Sublimate obtained from Cobalt, as above directed, is nothing but a metallic calx, that cannot be brought to the form and gloss of a metal, till it be worked up with fatty matters, as we shall shew in its place.

This calx is of a very singular nature, and differs from every other metallic calx, in that this is volatile, and all the rest extremely fixed; even those procured from the semi-metals: for the Flowers of Zinc, which are justly considered as a calcined Zinc, though obtained by a sort of sublimation, are not for all that of a volatile nature, but rather exceedingly fixed; seeing they are capable of sustaining the most violent fire, and melt instead of subliming. Arsenic, on the contrary, is not only extracted from its ore by sublimation, but when once sublimed continues to be volatile, and flies off in vapours as soon as it is exposed even to a moderate degree of heat.

This metallic matter, before it is combined with the phlogiston, is called White Arsenic, or plain Arsenic: it acquires the title of Regulus of Arsenic when it is united with the phlogiston, and glitters like a metal.

Though Arsenic be volatile, yet it requires a pretty strong fire to separate it from the minerals containing it, especially in close vessels; because it adheres very close to earthy and vitrifiable matters. This adhesion is so firm, that, when thus combined, it is capable of bearing a melting heat, and vitrifies with metallic calces, and other fusible matters. On this account it is impossible to extract from Cobalt, or other Arsenical matters, all the Arsenic they contain by working them only in close vessels. If such matters are to be freed from all their Arsenic, you must, after you have extracted all they will yield by distillation, put them into a crucible, and set it uncovered in the midst of a strong fire. Many Arsenical vapours will still rise; and care must be taken to stir the contents of the crucible frequently with an iron rod, to facilitate the discharge of the remaining Arsenic.

It often happens that the Arsenic, obtained from minerals by sublimation, is not very white, but of a lighter or darker grey colour. This is owing to some particles of inflammable matter, from which Arsenical minerals are seldom quite free. A very small quantity of phlogiston is sufficient to deprive much Arsenic of its whiteness, and to give it a grey colour. But when fouled in this manner, it may easily be brought to its due degree of whiteness: it need only be sublimed once more, after mixing it with some substance on which it doth not act; Sea-salt, for instance. If the matters from which Arsenic is extracted contain Sulphur also, as some pyrites do, the Arsenic sublimes with much less heat, than when it is united with earthy matters only; because it combines with the Sulphur, wherewith it hath a great affinity, and the Sulphur serves to separate the Arsenic, by this interposition, from the earth. In consequence hereof, Sulphur may be employed to extract Arsenic out of the earths in which it is fixed. In this case, the Sulphur changes the colour of the Arsenic, which it makes of a lighter or deeper yellow, or even red, in proportion to the quantity there is of it, and to the degree of fire that hath acted on both together.

The consistence of Arsenic is different, according to the degree of heat applied in subliming it. If the Arsenical vapour meet with a cold place, it gathers there in the form of a powder, as the Flowers of Sulphur do: this is the case with that which falls into the receiver in distilling it. But if it be stopped in a hot place, and cannot escape from that heat, it condenses into a heavy, compact, semi-transparent body, having undergone the first degree of fusion.

Yet it cannot be perfectly melted, so as to flow like other fused matters: not that it is refractory; for, on the contrary, the degree of heat in which it begins to melt is very moderate, and it is in its own nature very fit to promote the fusion of refractory matters: but the reason is this; it is necessarily converted into vapours by the degree of heat necessary to fuse it, and these vapours burst the vessels, if they find no vent.

Arsenic made yellow by a mixture of Sulphur, which is also called Orpiment, is reducible to the form of a solid Sublimate with more ease; because it is alloyed with a twentieth, or perhaps a tenth part, of its weight of Sulphur, which renders it more fusible.

Red Arsenic, which contains still more Sulphur, melts also more easily. It then becomes of a transparent red, like a ruby: and hence, when it is in this form, it is called Ruby of Arsenic.

When a combination of Sulphur and Arsenic is wanted, it is better to mingle and distil together such minerals as contain Sulphur and Arsenic, the white and the yellow pyrites, for instance, than to mingle pure Arsenic with pure Sulphur: for the great volatility of these two substances is a hindrance to their uniting; whereas, when combined with other matters, they are capable of sustaining a much greater degree of heat, which favours and promotes their union.

Those who work by the grate do not extract Arsenic out of Cobalt by distillation: they throw the ore mixed promiscuously with wood and charcoal into a great furnace, from whence a flue carries the vapours into a long winding passage, across which beams of wood are fixed at proper distances from each other. The Arsenical vapours being conducted into this passage, adhere both to the sides thereof and to the joists that lye across it. The fuliginous parts of the combustible matters being lighter ascend higher, and go out through a chimney at the farther end of this passage.

The Arsenic sublimed by this method is not white, but of a grey colour; owing to the inflammable matter of the wood and charcoal with which the ore is torrefied.

When all the Arsenic the Cobalt will yield is thus separated, the earthy fixed matter left behind is mixed with divers fusible matters and vitrified, and produces a glass of a beautiful blue colour. It is called Smalt. This glass is to be prepared in the following manner.

Take four parts of fine fusible sand, an equal quantity of any Fixed Alkali perfectly depurated, and one part of Cobalt from which the Arsenic hath been sublimed by torrefaction. Pulverize these different substances very finely, and mix them thoroughly together; put the mixture into a good crucible, cover it, and set it in a melting furnace. Make a strong fire, and keep it up constantly in the same degree for some hours. Then dip an iron wire into the crucible; to the end of which a glassy matter will stick, in the form of threads, if the fusion and vitrification be perfect. In this case take the crucible out of the fire; cool it by throwing water on it, and then break it. You will find in it a glass, which will be of an exceeding deep blue, and almost black, if the operation hath succeeded. This glass, when reduced to a fine powder, acquires a much brighter and more lively blue colour.

If you find after the operation that the glass hath too little colour, the fusion must be repeated a second time, with twice or thrice the quantity of Cobalt. If, on the contrary, the glass be too dark, less Cobalt must be used.

Instead of the mixture here prescribed you may employ a ready-made glass, providing it be white and fusible. But as glass is always hard to melt, and as the mixing Cobalt with it renders it still more refractory, therefore though an Alkaline Salt be one of the ingredients in its composition, it is proper to promote the fusion, by mixing therewith calcined wine-lees, in the quantity of one third part of the weight of the Cobalt.

In order to make the assay of a particular Cobalt, with a view to know what quantity of blue glass it will yield, it is necessary to perform the operation in the manner here set down; a great deal of time and trouble may be saved by melting one part of Cobalt with two or three parts of Borax. This Salt is very fusible, and turns, when melted, into a substance which, for a time, possesses all the properties of glass. In this trial the glass of Borax will be nearly of the same colour as the true glass, or Smalt, made with the same Cobalt.

The ores of Bismuth, as well as Cobalt, yield a matter that colours glass blue; nay, the Smalt made with these ores is more beautiful than that procured from the ore of pure Arsenic. Some Cobalts yield both Arsenic and Bismuth. When such Cobalts are used, it is common to find at the bottom of the crucible a little button of metallic matter, which is called Regulus of Cobalt. This Regulus is a sort of Bismuth, generally adulterated with a mixture of ferruginous and arsenical parts.

The heaviest and most fixed Flowers of Arsenic, procured from Cobalt, have likewise the property of giving a blue colour to glass. But this colour is faint: it is owing to a portion of the colouring matter carried up along with the Arsenic. These Flowers may be made an ingredient in the composition of blue glass, not only because of the colouring principle they contain, but also because they greatly promote fusion; Arsenic being one of the most efficacious fluxes known.

In short, all those blue glasses, or Smalts, contain a certain quantity of Arsenic; for a portion of this semi-metal always remains united with the fixed matter of the Cobalt, though roasted for a long time, and in a very hot fire. The portion of Arsenic that is thus fixed vitrifies with the colouring matter, and enters into the composition of the Smalt.

The blue glass made with the fixed part of Cobalt hath several names, according to the condition in which it is. When it hath undergone the first imperfect degree of fusion only it is called Zaffre. It takes the name of Smalt when perfectly vitrified: and this again being pulverized is called Powder-blue, or, if finely levigated, Blue Enamel; because it is used in enamelling, as well as in painting earthen ware and porcelain.

PROCESS II.

To separate Arsenic from Sulphur.

Powder the yellow or red Arsenic which you intend to separate from its Sulphur. Moisten this powder with a Fixed Alkali resolved into a liquor. Dry the mixture gently; put it into a very tall glass cucurbit, and fit on a blind-head. Set this cucurbit in a sand-bath; warm the vessels gently, and increase the fire by degrees, till you perceive that no more Arsenic sublimes. The Arsenic, which before was yellow or red, rises into the head partly in white flowers, and partly in a compact, white, semi-transparent matter, which looks as if it were vitrified. The Sulphur combined with the Fixed Alkali remains at the bottom of the cucurbit.

OBSERVATIONS.

A Fixed Alkali hath more affinity than any metallic substance with Sulphur: so that it is not surprising Sulphur should be separated from Arsenic by its interposition. Yet there is an inconvenience attends the use of it: for it hath a great affinity with the Arsenic also, and so always retains some part thereof, which continues fixed with it. For this reason care should be taken not to mix, with sulphurated Arsenic, a greater quantity of Alkali than is necessary to absorb the Sulphur it contains. Nothing, however, but experience and repeated trials can teach us the exact quantity of Alkali that ought to be employed; because the quantity of Sulphur that may be contained in yellow or red Arsenic is indefinite.

The vessel ought to be tall, that the upper part of the head, where the Arsenical particles condense, may be the less exposed to heat. Towards the end of the operation the fire must be strongly excited, so as to make the sand red-hot; because the last portions of Arsenic that rise are strongly retained by the Fixed Alkali.

Arsenic that is grey or blackish may be depurated and whitened by the same means; because a Fixed Alkali absorbs the phlogiston likewise with great avidity. Mercury, as well as a Fixed Alkali, is an excellent additament for separating Arsenic from Sulphur. If you will use it for that purpose, reduce the sulphurated Arsenic to a very fine powder, by rubbing it a long time in a glass mortar; when it is well pulverized, let a few drops of Mercury fall upon it, by squeezing it through chamoy, and continue the trituration. The yellow or red colour of the Arsenic will insensibly change, and gradually grow darker as the Mercury incorporates with it. When the Mercury is perfectly killed, add a little more of it than you did the first time, and in the same manner: continue to triturate till it disappear; and thus go on adding more and more till the Mercury you add remain quick, and you can kill no more of it. Neither the red nor the yellow colour will then appear in the mixture; which will be grey, if it contain but a little Sulphur, and black, if a great deal.

Put this mixture into a very tall glass cucurbit; fit on a blind-head; set it in a sand-bath, and bury it in the sand as far as the contained mixture reaches. Heat the vessels, and, during the whole operation, keep up a degree of fire a little weaker than that required for subliming Cinabar. White Arsenical Flowers will adhere to the upper part of the head, amongst which will be some beautiful crystals of Arsenic; and underneath them you will find some Cinabar sublimed, but not entirely free from Arsenic. If you desire to have your Cinabar and your Arsenic purer, and more unmixed with each other, separate the upper sublimate, which is Arsenical, from the lower, which consists chiefly of Cinabar. Powder each of them coarsely, and sublime them separately each in a different cucurbit.

On this occasion the Mercury separates the Sulphur from the Arsenic, because it hath a greater affinity than Arsenic with that mineral. It is not the only metallic substance of this character: for, as hath been shewn, there are several others that have a greater affinity than Mercury with Sulphur, being able to decompose Cinabar by their interposition. Yet those metallic substances must not be substituted for Mercury in the present operation: because there is none of them but hath at the same time a very great affinity with Arsenic, or even as strong an one as they have with Sulphur; whereas Mercury will by no means unite with Arsenic.

This method of separating Arsenic from Sulphur hath two advantages over that in which a Fixed Alkali is the medium. The first is, that by this means all the Arsenic contained in the mixture is extracted out of it; and the second, that, as Mercury doth not absorb Arsenic, we are not put to the trouble of groping out, as it were, by trials the quantity necessary to be added; and that, though more be added than is necessary to absorb all the Sulphur, it will be of no prejudice to the operation. But then it is attended with the inconvenience of being much more tedious and more laborious than the other. For, in the first place, it requires previously a very tiresome trituration, in order to procure an union between the Sulphur and the Mercury, and so to form an Æthiops; without which the Mercury and the sulphurated Arsenic will sublime separately, so that no decomposition will be effected. Secondly, though the Mercury be sufficiently united with the Sulphur of the Arsenic by the long trituration that precedes the sublimation, this doth not prevent, as we took notice above, the sublimed Arsenic and Cinabar from being in some measure blended together; so that each requires a second separate sublimation to render it very pure.

These inconveniencies cause a Fixed Alkali to be used preferably to Mercury; the loss of a small quantity of the Arsenic, which remains united with the Alkali, being little regarded; as that metallic substance is neither scarce nor precious.

When Arsenic is united with a great quantity of Sulphur, it may be freed from a part thereof without the intervention of any third body: it is sufficient for the purpose to sublime it with a very gentle fire, increased by insensible degrees. The most sulphureous part ascends first; what rises afterwards is more Arsenical, and less sulphureous; and the last flowers of all are pure Arsenic, or at least nearly so.

PROCESS III.

To give Arsenic the Metalline Form. Regulus of Arsenic.

Take two parts of white Arsenic in fine powder, one part of the black flux, half a part of Borax, and as much clean iron filings. Rub the whole together, in order to mix them thoroughly. Put this mixture into a good crucible, and over it put Sea-salt three fingers thick. Cover the crucible; set it in a melting furnace; and begin with a gentle fire to heat the crucible equally.

When arsenical vapours begin to ascend from the crucible, raise the fire immediately so as to melt the mixture. Examine whether or no the matter be thoroughly melted, by introducing an iron wire into the crucible; and if the fusion be perfect, take the crucible out of the furnace. Let it cool; break it; and you will find in it a Regulus of a white and livid metallic colour, very brittle, scarcely hard, but rather friable.

OBSERVATIONS.

White Arsenic is, as hath been said, a metallic calx; and consequently wants no more, in order to its acquiring the metalline properties, than to be combined with the phlogiston: this is effected by the operation before us.

The Iron added doth not serve here, as in making the Regulus of Antimony, to precipitate the Regulus of Arsenic, by separating it from some other substance with which it was united: on this occasion it does nothing but join the Regulus of Arsenic, to which it gives solidity and consistence. This is the only reason of its being made an ingredient in the mixture; as the Regulus of Arsenic, without it, would have such a tender consistence, that it could scarce be handled without falling asunder into little bits. The Iron procures a further advantage in this process; which is, that it prevents a great quantity of Arsenic from being lost in vapours: for the Arsenic, with which it combines, is restrained, and, in some measure, fixed by it.

Copper may be substituted for Iron, and procures the same advantages.

It is very necessary to remove the crucible from the fire as soon as the matter is melted, and indeed to cool it as expeditiously as possible, to prevent the Arsenic from flying off in vapours: for, when once the Regulus is formed, the proportion of Arsenic, with respect to that of the metal mixed with it, is continually lessening while it stays in the fire; so that, after some time, there will be left in the crucible, not a Regulus of Arsenic, but only Iron or Copper, alloyed with a little Arsenic. On this occasion the Copper turns white, and assumes the colour of Silver; but it soon tarnishes in the air.

It is easy to perceive, by what hath been said, that the Regulus of Arsenic made according to this process is never pure, but contains always a considerable quantity of Iron or Copper, whatever precautions be used: but it is difficult to avoid this inconvenience, for the reasons above assigned; and if we attempt to fuse Arsenic alone, with reducing fluxes, the greatest part thereof is dissipated in vapours, long before the very flux begins to melt: and that part of it, which is found metallized, is not collected in one mass at the bottom of the crucible, as in other metallic reductions; but in small particles, dispersed and mixed among the scoriæ. There are nevertheless several expedients for obtaining a Regulus of Arsenic absolutely pure, and unalloyed with any metallic substance.

First: into a little low cucurbit, covered with a blind-head, put Regulus of Arsenic made with Iron or Copper; set this cucurbit in a sand-bath; heat it till the sand begins to grow red, and you will see part of the Regulus sublime into the head, still retaining its metalline splendour. The portion of Regulus thus sublimed is pure Arsenic, or at least contains but a very small portion of the adventitious metal, which may have been carried up with it. What is left in the bottom of the cucurbit is the metal that was added, still containing a little Arsenic, which continues obstinately fixed with it, and which the violence of fire is unable to force away from it in close vessels.

Secondly: mix your Arsenic in equal parts with the black flux; put the mixture into such a cucurbit as that last mentioned; and apply to it the strongest degree of heat that can be procured by a sand-bath; arsenical flowers, of a blackish grey colour, will first sublime into the head, and after them a Regulus of Arsenic of a white metalline colour, which is pretty glossy, but tarnishes very soon in the air. This Regulus hath no solidity: it is exceedingly friable; but it is pure.

Thirdly: I have also made a Regulus of pure Arsenic by another method, which produces a much greater quantity thereof, with a much smaller degree of heat. For this purpose I powder the Arsenic, and mix with it any Fat Oil; so that the mixture may be like a liquid paste: this paste I put into a little phial of thin glass, like one of those used by apothecaries; I set this phial in a sand-bath, and gradually heat it, till the bottom of the pot containing the sand begin to be red. Part of the Oil first rises out of the phial in vapours, which must be suffered to pass off. After this the upper part of the phial is gradually lined, on the inside, with a glittering metallic crust, which makes it look like a quick-silvered glass. This crust is the Regulus of Arsenic. When it begins to sublime, the mouth of the phial must be slightly stopped with a bit of paper, and the heat increased a little, till you see that nothing more rises.

If you break the bottle after the operation, you will find its upper part crusted over with a coat of Regulus, thicker or thinner in proportion to the quantity of Arsenic employed. The Regulus is in a mass, of a beautiful brilliant colour, which to me seems to stand the air better than that of any Regulus made by other methods; probably because of the great quantity of fat matter with which it is united, and by which it is defended.

This Regulus of Arsenic is absolutely pure, and a much greater quantity thereof is obtained, by this method, than by treating it with the black flux; because the Arsenic is much sooner and more easily combined with the inflammable matter: and hence it comes to pass that part of the Arsenic doth not rise at first in grey flowers, as in operating with the black flux. Moreover, by our process, all the Arsenic is sublimed in Regulus: whereas, when the black flux is employed, a pretty considerable part of the Arsenic unites with the alkaline part of the flux, and remains fixed therewith. In our operation there is nothing left at the bottom of the phial, except an oily, light, but very fixed coal.

Regulus of Arsenic, in whatever manner made, may be easily reduced into white, crystalline Arsenic, by the means of a Fixed Alkali, or of Mercury, applied in the same manner as for separating Arsenic from Sulphur.

PROCESS IV.

To distil the Nitrous Acid by the interposition of Arsenic. Blue Aqua Fortis. A new Neutral Salt of Arsenic.

Pulverize finely any quantity you please of refined Salt-petre. Mix it accurately with an equal weight of white crystalline Arsenic, well pulverized, or else with very white and very fine flowers of Arsenic. Put this mixture into a glass retort, leaving one half of it empty. Set your retort in a reverberating furnace; apply a receiver having a small hole drilled in it, and containing a little filtered rain-water; lute the receiver to the retort with stiff lute. Begin with putting two or three small live coals in the ash-hole of the furnace, and replace them with others when they are ready to go out. Go on thus warming your vessels by insensible degrees, and put no coals in the fire-place, till the retort begin to be very warm. You will soon see the receiver filled with vapours of a dark-red, inclining to a russet colour. With a bit of lute stop the little hole of the receiver. The vapours will be condensed in the water of this vessel, and give it a very fine blue colour, that will grow deeper and deeper as the distillation advances. If your Salt-petre was not very dry, some drops of Acid will also come over, and falling from the nose of the retort mix with the water in the receiver. Continue your distillation, increasing the fire little by little as it advances, but exceeding slowly, till you see that when the retort is red-hot nothing more comes off; and then let your vessels cool.

When the vessels are cold, unlute the receiver, and, as expeditiously as you can, pour the blue aqua fortis it contains into a crystal bottle; which you must seal hermetically, because this colour disappears in a short time when the liquor takes air. You will find in the retort a white saline mass moulded in its bottom, and some flowers of Arsenic sublimed to its upper cavity, and into its neck.

Pulverize the saline mass, and dissolve it in warm water. Filter the solution, in order to separate some arsenical parts that will be left on the filter. Let the filtered liquor evaporate of itself in the open air; when it is sufficiently evaporated, crystals will shoot in it representing quadrangular prisms, terminated at each extremity by pyramids, that are also quadrangular. These crystals will be in confused heaps at the bottom of the vessel: over them will be other crystals in the form of needles; a saline vegetation creeping along the sides of the vessel; and the surface of the liquor will be obscured by a thin dusty pellicle.

OBSERVATIONS.

Arsenic, as we took notice in our Elements of the Theory, besides the properties it hath in common with metallic substances, possesses others also in common with saline substances. One of the most remarkable among the latter is that of decomposing Nitre; of expelling the Acid of that Salt from its Alkaline basis, assuming its place, and forming with that Alkali a Neutral Salt, which is very soluble in water, and shoots into regular crystals.

To inquire into what passes in the decomposition of Nitre by Arsenic, and into the new Salt resulting from thence, was the design of the first Memoir given in by me to the Academy of Sciences on this subject, and from that the present process is copied. Though the whole quantity of Arsenic prescribed in the process doth not enter into the composition of the new Neutral Salt, seeing some of it sublimes in flowers, that quantity must not therefore be thought too great: for we see, on the other hand, that part of the Nitre is not decomposed. The needle-like Salt is no other than Nitre that hath not suffered any decomposition, and actually deflagrates on live coals like common Nitre.

The precaution of putting some water in the receiver is absolutely necessary, to condense the nitrous vapours that rise in the distillation: for they are so elastic, so volatile, so dephlegmated, that a very small part of them will otherwise be condensed into a liquor, while the rest will remain in the form of vapours, to which vent must be given through the small hole in the receiver, as without that they will burst the vessels with impetuosity: and consequently scarce any Acid will be obtained; especially if the Nitre employed be very dry, as it must be to be reducible into a fine powder.

The blue colour communicated by the Nitrous Acid to the water is very remarkable. The cause that produces this colour is not yet known.

Though the Acid is, on this occasion, mortified by a great quantity of water, yet, when it rises out of the retort, it is so concentrated as to form, even with that water, if too much be not put in, a most active and even smoking aqua fortis.

It is necessary in this operation, and more so than in any other, to warm the vessels gradually, and to proceed exceeding slowly; otherwise the artist runs the risque of seeing his vessels burst to pieces with violence, and with great danger to his person: for Arsenic acts on Nitre with incredible vivacity; insomuch that, if a mixture of Nitre and Arsenic be heated to a certain degree, the Nitre is decomposed almost as rapidly, and with as great an explosion, as when it is made to fulminate with an inflammable matter. In short, the appearances are such, that one would be almost induced to think the Nitre really takes fire on this occasion: though it be only decomposed just as it is by the Vitriolic Acid.

The solution of the caput mortuum of this distillation contains, at the same time, several sorts of Salts: to wit, 1. the Neutral Salt of Arsenic, formed by the union of the Arsenic with the basis of the Nitre; this shoots into the prismatic crystals above-mentioned: 2. some Nitre that hath not been decomposed; this forms the needles and part of the vegetations: 3. a small portion of Arsenic, that is known to be soluble in water; this forms the thin dark pellicle that covers the surface of the liquor when it begins to evaporate.

For the properties of this new Neutral Salt of Arsenic you may consult what we have said thereupon in our Elements of the Theory, and in the Memoirs of the Academy of Sciences.

PROCESS V.

To alkalizate Nitre by Arsenic.

Melt in a crucible the Nitre you intend to alkalizate. When it is melted, and moderately red, project upon it two or three pinches of pulverized Arsenic. A considerable effervescence and ebullition will immediately be produced in the crucible, attended with a noise like that which Nitre makes, when it detonates with an inflammable matter. At the same time a thick smoke will rise, which at first will smell like garlic, the odour peculiar to Arsenic; it will also smell afterwards like Spirit of Nitre. When the effervescence in the crucible is over, throw again upon the Nitre as much pulverized Arsenic as you did the first time; and all the same phenomena will be repeated. Continue thus throwing in Arsenic in small parcels, till it produce no more effervescence; taking care to stir the matter at every projection with an iron wire, the better to mix the whole together. Then increase your fire, and melt what remains. Keep it thus in fusion for a quarter of an hour, and then take the crucible out of the fire. It will contain a Nitre alkalizated by Arsenic.

OBSERVATIONS.

This operation, as well as the preceding one, is a decomposition of Nitre by Arsenic; yet the result is very different: for, instead of a Salt capable of crystallizing, and discovering no tokens either of Acid or Alkali, we obtain, on this occasion, only a Salt that runs into a liquor by the moisture of the air, doth not crystallize, and hath all the properties of an Alkali.

These differences arise only from the different manner in which the decomposition of the Nitre, and the union of the Arsenic with the basis of that Salt, is brought about. When the Nitrous Acid is distilled by the interposition of Arsenic, with a view to obtain the Arsenical Salt, the operation must be performed in close vessels; no greater degree of heat must be applied to the mixture than is necessary for enabling the Arsenic to act; and that heat must be administered very slowly and by insensible degrees. But, when the business is to alkalizate Nitre by the means of Arsenic, the operation is performed in a crucible, in a naked fire, with a strong degree of heat, and that suddenly applied. The violence of the heat, the suddenness with which it is applied, the vivacity wherewith the Arsenic unites with the basis of the Nitre; and, still more than all these, the free access of the air, occasion the greatest part of the Arsenic, which at first combines with the basis of the Nitre after having expelled its Acid, to be presently carried off and dissipated in vapours; and consequently the basis of the Nitre, not being sufficiently saturated, discovers its Alkaline properties.

I say, the concurrence of the air contributes, still more than all the rest, to separate the Arsenic from the Alkaline basis of the Nitre; experience having taught me that the Neutral Salt of Arsenic is not to be alkalizated by the most violent force of heat, as long as it continues in close vessels, and the external air hath no communication with it; but that some of the Arsenic contained in that Salt is dissipated, by exposing it to a strong heat in open vessels.

The tumult and effervescence that arise, when Arsenic is projected on Nitre fused in a crucible, are so considerable, and so nearly resemble the detonation of Nitre with an inflammable matter, that we should be tempted to think, if we trusted appearances only, that Arsenic furnishes a combustible matter, and that the Alkalization of the Nitre is effected, on this occasion, in the same manner as when it is fixed by charcoal: but, by examining attentively what passes, we easily discover that there is no inflammation at all, and that the Nitre is alkalizated in the manner and by the means above pointed out.

The first vapours that rise, when Arsenic is projected on Nitre, are purely arsenical; and, if any cold body be put in their way, they adhere to it in the form of flowers. These vapours are actual particles of Arsenic, carried up by the heat before they could come to act on the Nitre; but they are soon after mixed with Nitrous vapours, consisting of the Acid of the Nitre, which the Arsenic expels from its basis as fast as it comes to act on that Salt.

The nearer you come to the end of the operation, the more does the matter in the crucible lose of its fluidity, though an equal fire be constantly kept up in the furnace. At last it becomes quite like a paste, and the fire must be made much stronger to put it again in fusion. The reason of this is, that Nitre when alkalizated is much less fusible than when it is not so. The case is the same when this Salt is alkalizated by deflagration.

Though the Nitre, when alkalizated, makes no more effervescence with Arsenic, and though, when kept in fusion, it emits no more arsenical vapours, it doth not thence follow that it is a pure Alkali, and that it contains no Arsenic: it still contains a large quantity thereof, but so strongly united that the force of fire is not able to separate them; which hath led some authors to give this Salt the title of Fixed Arsenic.

The existence of Arsenic in this saline compound is easily discovered, by fusing it with metallic substances, on which it produces the same effects as Arsenic.

With solutions of metals in the Acids, it also presents almost the same phenomena as the Neutral Salt of Arsenic. Particularly it precipitates Silver dissolved by the Nitrous Acid in a red powder, as that Salt does; and the differences observed between the precipitations made by our new Neutral Salt of Arsenic, and those made by Nitre alkalizated with Arsenic, can be attributed only to the alkaline quality of the latter. See the Memoirs of the Academy for 1746.

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