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SECTION II.. _of Operations On_ Metals.

Elements of the Theory and Practice of Chymistry, 5th Ed. · Pierre Joseph Macquer — chapter 39 of 43 · ~37,182 words · public domain

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Of Operations on METALS.

CHAP. I.

Of GOLD.

PROCESS I.

To separate Gold, by Amalgamation with Mercury, from the Earth and Stones with which it is found mixed.

Pulverize the earths and stones containing Gold. Put the powder into a little wooden tray; dip this tray in water, gently shaking it and its contents. The water will grow muddy, by taking up the earthy parts of the ore. Continue washing it in this manner till the water cease to appear turbid. Upon the ore thus washed pour strong vinegar, having first dissolved therein, by the help of heat, about a tenth part of its weight of alum. The powder must be quite drenched and covered with this liquor, and so left to stand for twice twenty-four hours.

Decant the vinegar, and wash your powder with warm water, till the last that comes off hath no taste: then dry it, and put it into an iron mortar, with four times its weight of Quick-silver: triturate the whole with a heavy wooden pestle, till all the powder be of a blackish colour: then pour in a little water, and continue rubbing for some time longer. More earthy and heterogeneous particles will be separated from the metalline parts by means of this water, which will look dirty: it must then be decanted, and more fair water added. Repeat this several times; then dry what remains in the mortar with a sponge, and by the help of a gentle heat: you will find it an Amalgam of the Mercury with the Gold.

Put this Amalgam into a chamoy bag: tie a knot on its neck, and squeeze it hard between your fingers, over some wide-mouthed vessel; there will issue through the pores of the leather numberless little jets of Mercury, forming a sort of shower, that will collect into large globules in the vessel placed underneath. When you can force out no more Mercury by this means, open the bag, and in it you will find the Amalgam freed from the superfluous Mercury; the Gold retaining only about as much thereof as nearly equals itself in weight.

Put this Amalgam into a glass retort; set this retort in the sand-bath of a reverberating furnace; cover it quite over with sand; apply a glass receiver half full of water, so that the nose of the retort may be under the water. The receiver need not be luted to the retort. Give a gradual heat, and raise the fire till drops of the sublimed Mercury appear in the neck of the retort, and fall into the water with a hissing noise. If you hear any noise in the retort slacken your fire a little. Lastly, when you observe, that, though you raise the fire still higher than before, nothing more will come over, take out your retort, break it, and there you will find the Gold, which must be melted in a crucible with Borax.

OBSERVATIONS.

Gold is a perfect metal, which can by no means be deprived of its Phlogiston, and on which few, even of the most powerful chymical solvents, have any effect: and therefore it almost always hath its metalline form when found in the earth; from which it may sometimes be separated by simple lotion. The Gold dust found in the sands of certain rivers is of this kind. When it resides in stones, or tenacious earths, it may be extracted by the process here delivered; to wit, by Amalgamation, or combination of Mercury with Gold. Mercury is incapable of uniting with any earthy substances, not even with the metallic earths, when they are deprived of their Phlogiston, and consequently have not the metalline form.

Hence it follows, that when Mercury is triturated with particles of Gold, of earth, and of stone, mingled together, it unites with the Gold, and separates it from those heterogeneous matters. Yet, if there be along with the Gold any other metal, in its metalline form, except Iron, the Mercury will amalgamate with that also. This often happens to Silver, which being a perfect metal as well as Gold, is for that reason sometimes dug up in its metalline form, and even incorporated with Gold. When this is the case, the mass that remains in the retort, after abstracting the Mercury of the Amalgama, is a compound of Gold and Silver, which are to be separated from each other by the methods we shall give for that purpose. The present process is therefore applicable to Silver as well as Gold.

Sometimes Gold is intimately combined with such mineral matters as hinder the Mercury from acting upon it. In that case the mixed mass must be roasted before you proceed to Amalgamation: for if the matters be volatile, such, for instance, as antimony or arsenic, the fire will carry them off; so that, after roasting, the Amalgamation will succeed. But sometimes these matters are fixed, and require fusion; if so, recourse must be had to some particular methods, which we shall describe when we come to treat of Silver, as these two perfect metals are to be treated in the same manner.

Ores containing Gold must be washed before an Amalgam is attempted; that the metalline parts, being freed from the numerous particles of earth with which they are encompassed, may the more readily incorporate with the Mercury. Besides, it is the property of Mercury to take the form of a dark unmetallic powder, after being long rubbed with other matters, so that it cannot be easily distinguished from the particles of earth. And hence, if you still continue to grind the matters together, after the Amalgamation is completed, and wash them again and again, the water that comes off will always look turbid, being impregnated with some particles of the Amalgam. This is easily proved: for if you let the turbid water settle, and distil the sediment, you will obtain Quick-silver from it.

The ore is to be steeped in vinegar charged with alum, in order to cleanse the surface of the Gold, which is often covered with a thin coat of earth that obstructs the Amalgamation.

Great care must be taken that the Mercury employed in this operation be very pure. If it be adulterated with any metallic substance, it must be freed therefrom by the methods which we shall propose in their proper place.

The way of separating Mercury from Gold is founded on the different properties of these two metallic substances; the one being exceedingly fixed, and the other very volatile. The union which Mercury contracts with the metals is not intimate enough, to give the new compound which results therefrom all the properties of either of the two united substances; at least so far as concerns their degrees of fixity and volatility. Hence it comes, that, in our Amalgam, the Gold communicates but very little of its fixity to the Mercury, and the Mercury communicates to the Gold but very little of its volatility. Yet if the Mercury be distilled off with a much greater degree of heat than is necessary to elevate it, a pretty considerable quantity of Gold will most certainly be carried up along with it.

It is also of consequence, on another account, that the fire be duly governed on this occasion. For if too great a degree of heat be applied, and the fire afterwards lowered, the water in the receiver, which covers the nose of the retort, will rise into its body, break it to pieces, and spoil the operation.

The cause of this phenomenon depends on the property which air possesses of rarefying with heat and condensing with cold, joined to its weight. As soon as the retort is acted on by a less degree of heat than acted on it the instant before, the air contained therein is condensed, and leaves a vacuum, which the external air, by virtue of its weight, tends to occupy; but, the orifice of the retort being under water, the external air can no way gain admittance, but by pushing in before it the water which intercepts its passage. This caution, as we observed above, must be applied to all distillations, where the vessels are disposed as they are in this.

Care must also be taken that the nose of the retort be not placed too deep under water: for as the neck grows very warm during the operation, because the degree of heat required to raise Mercury is about three times greater than that which raises water, it may easily be broken by the contact of the cold water in the receiver.

This method of extracting Gold and Silver from their ores, by Amalgamation with Mercury, is not to be absolutely depended on as a sure proof of the quantity of those metals that may be contained in the earth assayed by this means: for some small part of the Amalgam is always lost in washing it; and, moreover, the Mercury, when squeezed through chamoy, always carries with it a small portion of Gold. So that if you desire to know more exactly, by this method, the quantity of Gold or Silver contained in any earth, the Amalgam must not be squeezed through chamoy, but distilled altogether. Much the surest method of making an accurate assay is that by fusion and scorification, which we shall describe under the head of Silver.

In some countries, and especially in America, the method of Amalgamation is used for extracting Gold and Silver in large quantities, from the matrices which contain them in their metalline form. Agricola and other metallurgists have described the machines by means whereof such Amalgamations are managed.

PROCESS II.

To dissolve Gold in Aqua regis, and by that means to separate it from Silver. Aurum Fulminans. Aurum Fulminans reduced.

Take Gold that is perfectly pure, or alloyed with Silver only. Reduce it to little thin plates, by hammering it on an anvil. If it be not sufficiently tough, neal it till it be red in a moderate, clear fire, quite free from smoking coals, and then let it cool gradually, which will restore its ductility.

When the plates are thin enough, make them red hot once more, and cut them into small bits with a pair of sheers. Put these bits into a tall, narrow-mouthed cucurbit, and pour on them twice their weight of good Aqua regis, made of one part Sal Ammoniac, or Spirit of Salt, and four parts Spirit of Nitre. Set the cucurbit in a sand-bath moderately heated, stopping its orifice slightly with a paper coffin, to prevent any dirt from falling in. The Aqua regis will presently begin to smoke. Round the little bits of Gold will be formed an infinite number of small bubbles, which will rise to the surface of the liquor. The Gold will totally dissolve, if it be pure, and the solution will be of a beautiful yellow colour: if the Gold be alloyed with a small quantity of Silver, the latter will remain at the bottom of the vessel in the form of a white powder. If the Gold be alloyed with much Silver, when the Gold is dissolved the Silver will retain the form of the little metalline plates put into the vessel.

When the dissolution is completed, gently pour off the liquor into another low, wide-mouthed, glass cucurbit, taking care that none of the Silver, which lies at the bottom in the form of a powder, escape with the liquor. On this powder of Silver pour as much fresh Aqua regis as will cover it entirely; and repeat this till you are sure that nothing more can be taken up by it. Lastly, having decanted the Aqua regis from the Silver, wash the Silver with a little Spirit of Salt weakened with water, and add this Spirit of Salt to the Aqua regis in which your Gold is dissolved. Then to the body containing these liquors fit a head and a receiver, and distil with a gentle heat, till the matter contained in the cucurbit become dry.

OBSERVATIONS.

It is certain that aqua regis is the true solvent of Gold, and that it does not touch Silver: so that if the Gold dissolved in it were alloyed with Silver, which is often the case, the two metals would by this means be pretty accurately separated from each other. But if you desire to obtain from this solution a Gold absolutely pure, you must free it, before you dissolve it, from every other metallic substance but Silver; because aqua regis acts upon most of the other metals and the semi-metals. We shall shew under the head of Silver, as we promised before, how to purify a mass of Gold and Silver from every other metallic alloy. Thither also we refer the common parting assay performed by means of aqua fortis: because in that operation the Silver is dissolved, and not the Gold.

If the Gold put to dissolve in aqua regis be pure, the dissolution is easily and readily effected. But if, on the contrary, it be alloyed with Silver, the aqua regis finds more difficulty in dissolving it. Nay, if the Silver exceed the Gold in quantity, the dissolution will not take place at all, for the reasons adduced in our Theoretical Elements; of which we shall speak more fully when we come to treat of the Parting Assay.

In the process we directed the Gold to be dissolved in a tall body. This precaution is necessary to prevent the loss of some part thereof: for it is the property of aqua regis to carry off along with it some of the Gold, especially when there is any Sal Ammoniac in its composition, if the vessel be heated while the dissolution is going on, or if the aqua regis be very strong. Yet it is proper to make use of aqua regis that is too strong rather than too weak: for if it prove too strong, and be observed not to act upon the metal for that reason, it is easy to weaken it, by gradually adding small quantities of pure water, till you perceive it begin to act with vigour. This is a general rule regarding all metallic dissolutions in Acids.

When the solution of Gold is evaporated to dryness, if you desire to reduce into a mass the Gold dust left at the bottom of the cucurbit, you must put it into a crucible, and cover it with pulverized borax, mixed with a little nitre and calcined wine-lees; then cover the crucible close, heat it with a moderate fire, which must be afterwards increased so as to melt the contents. At the bottom of the crucible you will find a lump of Gold, over which the salts you added will be as it were vitrified. These salts are added chiefly to promote the fusion of the metal.

The Gold may, if you will, be separated from its solvent without evaporating the solution as above directed. You need only mix with the solution a fixed or volatile Alkali by little and little, till you see no more precipitate fall, and then let the liquor stand to settle, at the bottom of which you will find a sediment: filter the whole, and dry what is left on the filter.

Both fixed and volatile Alkalis possessing, as hath been frequently repeated, a greater affinity with Acids than metallic substances have, they precipitate the Gold, and separate it from the Acids in which it is dissolved: but it is of great consequence to take notice, that, if you attempt to melt this precipitated Gold in a crucible, it will fulminate as soon as it feels the heat, with such a terrible explosion, that, if the quantity be at all considerable, it may prove fatal to the operator: even rubbing it a little hard will make it blow up. This preparation is therefore called Aurum Fulminans.

Hitherto no satisfactory explanation hath been given of this phenomenon. Some Chymists considering, that, in the precipitation of the Gold, a Nitre is regenerated by the union of the Alkali with the Nitrous Acid which enters into the composition of the aqua regis, imagine that some of this regenerated Nitre, combining with the precipitated Gold, takes fire and detonates, either by means of some small portion of Phlogiston that may be contained in the Alkali, or by means of that which constitutes the Gold itself. But, in the first place, it is well known that Fixed Alkalis do not contain Phlogiston enough to make Nitre detonate. Indeed, if a Volatile Alkali be employed in the precipitation, a Nitrous Ammoniacal Salt will be formed, containing Phlogiston enough to be capable of detonating without the concourse of any additional Phlogiston: but this detonation of the Nitrous Ammoniacal Salt is not to be compared, as to the violence of its effects, with the fulmination of Gold. Besides, we do not find that Gold precipitated by a Volatile Alkali explodes with greater force than that precipitated by a Fixed Alkali. As for the Gold, it is certain that it suffers no decomposition at all by fulminating. When fulminated under a glass bell, in such small quantities as not to endanger the operator, the Gold is found scattered about under the bell in very fine particles, without having undergone any alteration.

Others have fancied this fulmination of the Gold to be nothing but the decrepitation of the Sea-salt that is regenerated, in the precipitation of the metal, by the Fixed Alkali uniting with the Acid of Sea-salt which makes part of the aqua regis. But to this it may be said, that Gold precipitated by a Volatile Alkali fulminates as violently as that precipitated by a Fixed Alkali; and yet no sea-salt can be formed in the liquor by the addition of a Volatile Alkali, but only a Sal Ammoniac which has not the property of decrepitating. Moreover, there is no comparison, as to the effects, between the decrepitation of Sea-salt and the fulmination of Gold.

Nor, lastly, can this fulmination be attributed, as it is by some, to the effort made by the Salts to escape from amidst the particles of Gold, in which they are supposed by them to be imprisoned: for then we might deprive this Gold entirely of its fulminating quality by only boiling it in water, and so washing off all the saline particles, which probably adhere to its surface only. It is plain there is great room for very beautiful discoveries on this subject. In Walerius's Mineralogy we find some observations that may throw a little light on the point before us.

"The quantity," says he, "of fulminating Gold precipitated exceeds that of the Gold dissolved: if the aqua regis be made with Sal Ammoniac the explosion will be stronger; it will also be more violent if the solution be precipitated with a Volatile Alkali, than if a Fixed Alkali be used for that purpose."

One of the speediest and easiest methods to deprive this Gold of its fulminating quality, is to grind in a mortar twice as much flowers of Sulphur as you have Gold to reduce, mixing your fulminating Gold therewith by little and little, as you grind them together; then to put the mixture into a crucible, and heat it just enough to melt the Sulphur. Part of the Sulphur will be dissipated in vapours, and the rest will burn away. When it is quite consumed, increase the fire so as to make the crucible red-hot. When you perceive no more smell of Sulphur, pour on the Gold a little Borax, previously melted in another crucible with a Fixed Alkali, as calcined Wine-lees, or Nitre fixed with Tartar; and then raise the fire sufficiently to make the whole flow. After the fusion is completed, you will find a button of Gold at the bottom of the crucible under the Salts.

Fulminating Gold may also be reduced by pouring on it a sufficient quantity of Fixed Alkali reduced to a liquor, or of oil of Vitriol, evaporating all the moisture, and gradually throwing what remains, mixed up with some pinguinous matter, into a crucible kept red-hot in a furnace. The reason why these substances deprive the Gold of its fulminating quality, depends on the causes that produce the fulmination.

Gold may also be separated from aqua regis, and precipitated by the means of several metallic substances that have a greater affinity, either with aqua regis, or with one of the two Acids that compose it. Mercury is one of the fittest for this purpose. On dropping a solution of Mercury in the Nitrous Acid by little and little into a solution of Gold, the mixture becomes turbid, and a precipitate is formed. Continue dropping in more of the solution of Mercury till no more precipitate falls; then let the liquor stand to settle, and at the bottom of it you will find a sediment, which is the precipitated Gold: pour off the liquor by inclination, and wash the precipitate with fair water.

Mercury hath a greater affinity with the Marine than with the Nitrous Acid. The affinity which Mercury hath with the Marine Acid is also greater than that of Gold with the Marine Acid; for unless this Acid be associated either with the Nitrous Acid, or at least with a certain proportion of Phlogiston, it will not dissolve Gold. Hence it comes, that when a solution of Mercury in the Nitrous Acid is dropped into a solution of Gold in aqua regis, the Mercury unites with the Acid of Sea-salt, which is an ingredient in the aqua regis: but the Marine Acid cannot on this occasion join the Mercury, without deserting the Gold and the Nitrous Acid with which it was united; and then the Gold, which cannot be kept in solution by the Nitrous Acid alone, is forced to quit its solvent and precipitate. The liquor, therefore, that now floats over the Gold thus precipitated, must contain Mercury united with the Acid of Sea-salt: and in fact it yields a true Corrosive Sublimate, which is known to be a combination of Mercury with the Marine Acid.

Mercury dissolved in Spirit of Nitre is employed to procure the precipitation we are speaking of; because metallic substances, when so comminuted by an Acid, are much fitter for such experiments than when they are in a concrete form.

Gold precipitated in this manner by a metallic substance doth not fulminate.

PROCESS III.

To dissolve Gold by Liver of Sulphur.

Mix together equal parts of common Brimstone, and a very strong Fixed Alkali; for instance, Nitre fixed by Charcoal. Put them in a crucible, and melt the mixture, stirring it from time to time with a small rod. There is no occasion to make the fire very brisk; because the Sulphur facilitates the fusion of the Fixed Alkali. Some sulphureous vapours will rise from the crucible; the two substances will mix intimately together, and form a reddish compound. Then throw into the crucible some little pieces of Gold beat into thin plates, so that the whole do not exceed in weight one third part of the Liver of Sulphur: raise the fire a little. As soon as the Liver of Sulphur is perfectly melted, it will begin to dissolve the Gold with ebullition; and will even emit some flashes of fire. In the space of a few minutes the Gold will be entirely dissolved, especially if it was cut and flatted into small thin leaves.

OBSERVATIONS.

The process here delivered is taken from M. Stahl. The design of that ingenious Chymist's inquiry was to discover how Moses could burn the golden calf, which the Israelites had set up and worshipped while he was on the mount; how he could afterwards reduce that calf to powder, throw it into the water which the people used, and make all who had apostatized drink thereof, as related in the Book of Exodus.

M. Stahl, having first observed that Gold is absolutely unalterable and indestructible by the force of fire alone, be it ever so violent, concludes, that without a miracle Moses could not possibly perform the above-mentioned operations on the golden calf any way but by mixing with the Gold some matter qualified to alter and dissolve it. He then takes notice, that pure Sulphur does not act upon Gold at all, and that many other substances, which are thought capable of dividing and dissolving it, cannot however do it so completely as is necessary to render that metal susceptible of the effects related. He then gives the method of dissolving it by Liver of Sulphur, described in the process.

Liver of Sulphur dissolves likewise all the other metals: but M. Stahl observes, that it attenuates Gold more than any other metallic substance, and unites with it much more intimately than with the rest. This appears from what happens, on attempting to dissolve in water any of the mixts resulting from the union of another metal with the Liver of Sulphur: for then the metal separates, and appears in the form of a powder or fine calx; whereas, when Gold is united with Liver of Sulphur, the whole compound dissolves in water so perfectly, that the Gold even passes with the Liver of Sulphur through the pores of filtering paper.

If an Acid be poured into a solution of this combination of Gold with Liver of Sulphur, the Acid unites with the Alkali of the Hepar, and the Gold falls to the bottom of the liquor along with the Sulphur, which doth not quit it. The Sulphur thus precipitated with the Gold is easily carried off by a slight torrefaction, after which the Gold remains exceedingly comminuted. The Sulphur of this compound may also be destroyed by torrefaction, without the trouble of a previous solution and precipitation, and then also the Gold remains so attenuated as to be miscible with liquors, and floats on them, or swims in them, in such a manner that it may easily be swallowed with them in drinking. From all this M. Stahl concludes there is great reason to believe it was by means of the Liver of Sulphur that Moses divided, and in a manner calcined, the golden calf, so that he could mingle it with water, and make the Israelites drink it.

PROCESS IV.

To separate Gold from all other metallic Substances by means of Antimony.

Having put the Gold you intend to purify into a crucible, set it in a melting furnace, cover it, and make the Gold flow. When the metal is in fusion cast upon it, by a little at a time, twice its weight of pure crude Antimony in powder, and after each projection cover the crucible again immediately: this done keep the matter in fusion for a few minutes. When you perceive that the metallic mixture is perfectly melted, and that its surface begins to sparkle, pour it out into a hollow iron cone, previously heated, and smeared on the inside with tallow. Immediately strike with a hammer the floor on which the cone stands; and when all is cold, or at least sufficiently fixed, invert the cone and strike it: the whole metallic mass will fall out, and the under part thereof, which was at the point of the cone, will be a Regulus more or less yellow as the Gold was more or less pure. On striking the metallic mass the Regulus will freely part from the sulphureous crust at top.

Return this Regulus into the crucible, and melt it. Less fire will do now than was required before. Add the same quantity of Antimony, and proceed as at first. Repeat the same operation a third time, if your Gold be very impure.

Then put your Regulus into a good crucible, much larger than is necessary to hold it. Set your crucible in a melting furnace, and heat the matter but just enough to make it flow, with a smooth, brilliant surface. When you find it thus conditioned, point towards it the nose of a long-snouted pair of bellows, and therewith keep gently and constantly blowing. There will arise from the crucible a considerable smoke, which will abate greatly when you cease to blow, and increase as soon as you begin again. You must raise the fire gradually as you approach towards the end of the operation. If the surface of the metal lose its brilliant polish, and seem covered with a hard crust, it is a sign the fire is too weak; in which case it must be increased, till the surface recover its shining appearance. At last, when no more smoke rises, and the surface of the Gold looks neat and greenish, cast on it, by little and little, some pulverized Nitre, or a mixture of Nitre and Borax. The matter will swell up. Continue thus adding more Nitre gradually, till no commotion is thereby produced in the crucible; and then let the whole cool. If you find, when the Gold is cold, that it is not tough enough, melt it over again; when it begins to melt, cast in the same Salts as before; and repeat this till it be perfectly ductile.

OBSERVATIONS.

Antimony is a compound, consisting of a semi-metallic part united with about a fourth part of its weight of common Sulphur. It appears, in the ninth column of the Table of Affinities, that all the metals, Mercury and Gold excepted, have a greater affinity than the reguline part of Antimony with Sulphur. If therefore Gold, adulterated with a mixture of Copper, Silver, or any other metal, be melted with Antimony, those metals will unite with the Sulphur of the Antimony, and separate it from the reguline part, which being thus set free will combine and be blended with the Gold. These two metallic substances, forming a mass far heavier than the other metals mixed with the sulphur, fall together to the bottom of the crucible in the form of a Regulus, while the others float over them like a sort of scoria or flag: and thus the Gold is freed from all alloy but the reguline part of the Antimony.

As all the other metals have a great affinity with Sulphur, and Gold is the only one that is capable of resisting its action, one would think Sulphur alone might be sufficient to free it from the metals combined with it, and that it would therefore be better to employ pure Sulphur, in this operation, than to make use of Antimony; the reguline part of which remaining united with the Gold requires another long and laborious operation to get rid of it.

Indeed, strictly speaking, Sulphur alone would be sufficient to produce the desired separation: but it is proper to observe, that, as Sulphur alone is very combustible, most of it would be consumed in the operation before it could have an opportunity to unite with the metallic substances; whereas, when it is combined with the Regulus of Antimony, it is thereby enabled to bear the action of the fire much longer without burning, and consequently is much fitter for the purpose in question. Besides, if we were to make use of pure Sulphur, a great part of the Gold, which is kept in perfect fusion, and its precipitation facilitated, by the Regulus of Antimony, would remain confounded with the Sulphureous scoria.

Nevertheless, seeing the metals with which Gold is alloyed cannot be separated from it by Antimony, but that a quantity of Regulus proportioned to the quantity of the metals so separated will unite with the Gold, and that the more Regulus combines with the Gold, the more tedious, chargeable, and laborious will the operation prove, this consideration ought to have some influence in directing our process. Therefore, if the Gold be very impure, and worse than sixteen carats, we must not mix it with crude Antimony alone, but add two drams of pure Sulphur for every carat the Gold wants of sixteen, and lessen the quantity of Antimony in proportion to that of the real Gold.

It is necessary to keep the crucible close covered, after mixing the Antimony with the Gold, to prevent any coals from falling into it: for, if that should happen, the melted mass would puff up considerably, and might perhaps run over.

The inside of the cone, into which you pour the melted metallic mass, must be greased with tallow, to prevent its sticking thereto, and that it may come easily out. Striking the floor, on which the cone with the melted metal stands, helps the precipitation and descent of the Regulus of Gold and Antimony to the bottom of the cone.

Less fire is requisite to melt this compound Regulus, in order to add fresh Antimony, than was necessary before the Gold was mixed with the reguline part of the Antimony; because this metallic substance, being much more fusible than Gold, promotes its melting. The Antimony is mixed with the Gold by repeated projections, that the separation of the metals may be accomplished with the greater ease and accuracy. Yet the operation might be successfully performed, by putting in all the Antimony at once, and with one melting only.

The metalline mass found at the bottom of the cone after all these operations, is a mixture of Gold with the reguline part of the Antimony. All the rest of the process consists only in separating this reguline part from the Gold. As Gold is the most fixed of all metals, and as the Regulus of Antimony cannot bear the violence of fire without flying off in vapours, nothing more is necessary for this purpose but to expose the compound, as directed in the process, to a heat strong enough and long enough continued, to dissipate all the Regulus of Antimony. This semi-metal exhales in the form of a very thick white smoke. It is proper to blow gently into the crucible during the whole operation; because the immediate contact of the fresh air incessantly thrown in promotes and considerably increases the evaporation: and this is a general rule applicable to all evaporations.

The fire must be gradually raised as the Regulus of Antimony is dissipated, and the operation draws towards an end; because the mixed mass of Regulus of Antimony and Gold becomes so much the less fusible as the proportion of the Regulus is lessened. Though the Regulus of Antimony be separated from the Gold in this operation, because the latter is of such a fixed nature that it cannot be volatilized by the degree of fire which dissipates the Regulus; yet, as the Regulus is very volatile, it will undoubtedly carry up some of the Gold along with it, especially if you hurry on the evaporation too fast, by applying too great a degree of fire, by blowing too briskly into the crucible, and still more if you evaporate your mixture in a broad flat vessel instead of a crucible. All these things must therefore be avoided, if you would lose no more Gold than you needs must.

However, unless the evaporation be carried to the utmost, by the means above pointed out, a small portion of the Regulus of Antimony will always remain combined with the Gold, which defends it from the action of the fire. This small portion of Regulus hinders the Gold from being perfectly pure and ductile. In order therefore to consume and scorify it, we cast Nitre into the crucible when we perceive it to emit no more white vapours.

We know that Nitre has the property of reducing all metallic substances to a calx, Gold and Silver excepted; because it deflagrates with the phlogiston to which their metalline form is owing: but as this accension of the Nitre occasions a tumid effervescence, care must be taken to throw it in but by little and little at a time; for if too much be projected at once the melted matter will run over.

This operation might be considerably abridged by taking advantage of the property which Nitre possesses of thus consuming the phlogiston of metallic substances; as by means thereof we might destroy all the Regulus of Antimony incorporated with the Gold, without having recourse to a long and tedious evaporation. But then we should at the same time lose a much greater quantity of Gold, by reason of the tumult and ebullition which are inseparable from the detonation of Nitre. On the whole, therefore, if Nitre be made use of to purify Gold, great care must be taken to apply but very little of it at a time.

All the Silver that was mixed with the Gold, and indeed a little of the Gold itself, remains confounded with the sulphureous scoria, which floats upon the Golden Regulus after the addition of the Antimony: we shall shew in the Chapter on Silver how these two metals are to be separated from the Sulphur.

CHAP. II.

Of SILVER.

PROCESS I.

To separate Silver from its Ore, by means of Scorification with Lead.

Beat to powder in an iron mortar the ore from which you mean to separate the Silver, having first roasted it well in order to free it from all the Sulphur and Arsenic that it may contain. Weigh it exactly: then weigh out by itself eight times as much granulated Lead. Put one half of this Lead into a test, and spread it equally thereon: upon this Lead lay your ore, and cover it quite over with the remaining half of the Lead.

Place the test thus loaded under the further end of the muffle in a cupelling furnace. Light your fire, and increase it by degrees. If you look through one of the apertures in the door of the furnace you will perceive the ore, covered with calcined Lead, swim upon the melted Lead. Presently afterwards it will grow soft, melt, and be thrown towards the sides of the vessel, the surface of the Lead appearing in the midst thereof bright and shining like a luminous disc: the Lead will then begin to boil, and emit fumes. As soon as this happens, the fire must be a little checked, so that the ebullition of the Lead may almost entirely cease, for about a quarter of an hour. After this it must be excited to the degree it was at before, so that the Lead may begin again to boil and smoke. Its shining surface will gradually lessen, and be covered with scoriæ. Stir the whole with an iron hook, and draw in towards the middle what you observe towards the sides of the vessel; to the end that, if any part of the ore should still remain undissolved by the Lead, it may be mixed therewith.

When you perceive that the matter is in perfect fusion, that the greatest part of what sticks to the iron hook, when you dip it in the melted matter, separates from it again, and drops back into the vessel; and that the extremity of this instrument, when grown cold, appears varnished over with a thin, smooth, shining crust; you may look on these as marks that the business is done, and the more uniform and evenly the colour of the crust is, the more perfect may you judge the scorification to be.

Matters being brought to this pass, take the test with a pair of tongs from under the muffle, and pour its whole contents into an iron cone, first heated and greased with tallow. This whole operation lasts about three quarters of an hour. When all is cold, the blow of a hammer will part the Regulus from the scoria; and as it is not possible, how perfect soever the scorification be, to avoid leaving a little Lead containing Silver in the scoria, it is proper to pulverize this scoria, and separate therefrom whatever extends under the hammer, in order to add it to the Regulus.

OBSERVATIONS.

Silver, as well as Gold, is often found quite pure, and under its metalline form, in the bowels of the earth; and in that case it may be separated from the stones or sand in which it is lodged by simple washing, or by Amalgamation with Mercury, in the same manner as before directed for Gold. But it also happens frequently, that Silver is combined in the ore with other metallic substances and minerals, which will not admit of this process, but force us to employ other methods of separating it from them.

Sulphur and Arsenic are the substances to which Silver and the other metals usually owe their mineral state. These two matters are never very closely united with Silver; but may be pretty easily separated from it by the action of fire, and the addition of Lead. If Arsenic be predominant in a Silver ore, it will unite with the Lead by the help of a pretty moderate heat, and quickly convert a considerable quantity thereof into a penetrating fusible glass, which has the property of scorifying with ease all substances that are capable of scorification.

When Sulphur predominates, the scorification proceeds more slowly, and doth not always succeed; because that mineral combined with Lead lessens its fusibility, and retards its vitrification. In this case, part of the Sulphur must be dissipated by roasting: the other part unites with the Lead; and that, being rendered lighter by this union, floats on the rest of the mixture, which chiefly contains the Silver. At last, the joint action of the air and of the fire dissipates the portion of Sulphur that had united with the Lead: the Lead vitrifies and reduces to a scoria whatever is not either Silver or Gold: and thus the Silver being disentangled from the heterogeneous matters with which it was united, one part thereof being dissipated and the other vitrified, combines with the portion of Lead which is not vitrified, and falls through the scoria, which, to favour its descent, must be in perfect fusion.

The whole process, therefore, consists of three distinct operations. The first is Roasting, which dissipates some of the volatile substances found united with the Silver: the second is Scorification, or the Vitrification of the fixed matters also united with the Silver, such as sand, stones, metals, &c. and the third is precipitation, or the separation of the Silver from the scoria. The two first are, as hath been shewn, preparatives for the last, and indeed produce it.

As every thing we said concerning Gold, when we treated of the process of Amalgamation, is to be applied to Silver, which may be extracted by the same method when it is in its metalline form; in the same manner, all we now advance touching the method of extracting Silver by Scorification, when it is depraved with a mixture of heterogenous matters, is equally applicable to Gold in the same circumstances: and indeed Silver almost always contains more or less Gold naturally.

In the process we directed, that the ore should be pulverized before it be exposed to the fire, with a view to enlarge its surface, and by that means facilitate the action of the Lead upon it, as well as the evaporation of its volatile parts.

We recommended the precaution of slackening the fire a little at the beginning of the operation, only to prevent the Lead from being too hastily converted into litharge, lest it should penetrate and corrode the test before it had wholly dissolved the ore: but if we were perfectly certain of the vessel's being so good as to be in no danger of penetration by the Lead, this precaution would be needless.

It is proper to add eight parts of Lead for one of ore; though so much is not always absolutely necessary, especially when the ore is very fusible. The success of this operation depends chiefly on the completeness of the Scorification; and therefore the addition of more Lead than enough is attended with no inconvenience: for, as it always promotes the Scorification, it can never do any harm.

If the ore be mixed with such earthy and stony parts as cannot be separated from it by washing, it is the more difficult of fusion, even though the stones should be such as are most disposed to vitrify; because the most fusible earths and stones are always less so than most metallic substances. In that case it will be necessary, for effecting the Scorification, to mix thoroughly with the pulverized ore an equal quantity of Glass of Lead, to add twelve times as much granulated Lead, and then to proceed as directed for a fusible ore; exposing the mixture to a degree of fire strong enough, and long enough kept up, to give the scoria all the properties above required as signs of a perfect scorification.

Silver ore is sometimes mixed with Pyrites, and the ore of Arsenic, or Cobalt, which also make it refractory. As the Pyrites contain a large quantity of Sulphur, which is very volatile as well as Arsenic; in this case it is proper to begin with freeing the ore from these two extraneous substances. This is easily done by roasting: only be sure, when you first expose the ore to the heat, to cover the vessel in which you roast it, for some minutes, with an inverted vessel of the same width; because such sorts of ore are very apt to fly when they first feel the heat.

After this uncover it, and leave it exposed to the fire till no more sulphureous or arsenical matters rise. Then mix it with the same quantity of Glass of Lead as we ordered for ores rendered refractory by the admixture of earths or stones, and proceed in the same manner.

It is the more necessary to roast Silver ore infected with Sulphur and Arsenic, because, as Sulphur obstructs the fusion of Lead, it cannot but do hurt, and protract the operation; and Arsenic does mischief, on the other hand, by scorifying a very great quantity of Lead too hastily.

When the Sulphur and Arsenic are dissipated by roasting, the ore must be treated like that which is rendered refractory by stony and earthy matters; for as the pyrites contain much iron, there remains, after the Sulphur is evaporated, a considerable quantity of martial earth, which is difficult to scorify. The pyrites, as well as the cobalts, contain moreover an unmetallic earth, which is hard to fuse.

The general rule therefore is, when the ore is rendered refractory by any cause whatever, to mix it with Glass of Lead, and to add a larger quantity of granulated Lead. Yet some ores are so refractory that Lead alone will not do the business, and recourse must be had to some other flux. That which is fittest for the present purpose is the Black Flux, composed of one part of Nitre and two parts of Tartar deflagrated together. The Phlogiston contained in this quantity of Tartar is more than sufficient to alkalizate the Nitre. This Flux, therefore, is nothing more than Nitre alkalizated by Tartar, mixed with some of the same Tartar that hath not lost its Phlogiston, and is only reduced to a sort of coal.

The White Flux is also very fit to promote fusion; but on this occasion the Black Flux is preferable, because the Phlogiston of the Black Flux prevents the Lead from being too soon converted to litharge, and so gives it time to dissolve the metallic matters. The White Flux, which is the result of equal parts of Tartar and Nitre alkalizated together, being no more than an Alkali destitute of Phlogiston, or containing but very little, doth not possess this advantage.

If Silver should be combined in the ore with Iron in its metalline state, which however does not commonly happen, then, in order to separate them, the Iron must be deprived of its Phlogiston, and converted to a crocus before the mixed mass be melted with Lead; which may be done by dissolving it in the Vitriolic Acid, and then evaporating the Acid.

We are necessitated to make use of this contrivance, because Iron in its metalline form cannot be dissolved either by Lead or by the Glass of Lead; but when it is reduced to a calx, litharge unites with it and scorifies it.

If you have not at hand the utensils necessary for performing the operation we have been describing in a test, and under the muffle; or if you have a mind to work on a greater quantity of ore at a time, you may make use of a crucible for the purpose, and perform the operation in a melting furnace.

In this case the ore must be prepared, as above directed, according to its nature, and mixed with a proper quantity of Lead and Glass of Lead; the whole put into a good crucible, leaving two thirds thereof empty, and covered with a mixture of Sea-salt and a little Borax, both very dry, to the thickness of a full half inch.

This being done, set the crucible in the midst of a melting furnace, raise the coals quite to the lip of the crucible; light the fire; cover the furnace with its dome; but do not urge the fire more than is necessary to bring the mixture to perfect fusion: leave it thus in fusion for a good quarter of an hour; stir the whole with a bit of strong iron wire; then let it cool; break the crucible, and separate the Regulus from the scoria.

The Salts added on this occasion are fluxes, and their use is to procure a perfect fusion of the scoria.

If the melted matters be left exposed to the fire, either in a test or in a crucible, longer than is above prescribed, the portion of Lead, that hath united and precipitated with the Silver, will at last vitrify, and at the same time scorify all the alloy with which that metal may be mixed. But as there are no vessels that can long endure the action of litharge, without being pierced like a sieve, some of the Silver may escape through the holes or fissures of the vessel, and so be lost. It is better, therefore, to complete the purification of your Silver by the operation of the Cupel, the description of which follows.

PROCESS II.

The refining of Silver by the Cupel.

Take a cupel capable of containing one third more matter than you have to put into it: set it under the muffle of a furnace, like that described in our Theoretical Elements, as peculiarly appropriated to this sort of operation. Fill the furnace with charcoal; light it; make the cupel red-hot, and keep it so till all its moisture be evaporated; that is, for about a good quarter of an hour, if the cupel be made wholly of the ashes of burnt bones; and for a whole hour, if there be any washed wood-ash in its composition.

Reduce the Regulus which remained after the preceding operation to little thin plates, flatting them with a small hammer, and separating them carefully from all the adherent scoria. Wrap these in a bit of paper, and with a small pair of tongs put them gently into the cupel. When the paper is consumed the Regulus will soon melt, and the scoria, which will be gradually produced by the Lead as it turns to litharge, will be driven to the sides of the cupel, and immediately absorbed thereby. At the same time the cupel will assume a yellow, brown, or blackish colour, according to the quantity and nature of the scoria imbibed by it.

When you see the matter in the cupel in a violent ebullition, and emitting much smoke, lower the fire by the methods formerly prescribed. Keep up such a degree of heat only that the smoke which ascends from the matter may not rise very high, and that you may be able to distinguish the colour which the cupel acquires from the scoria.

Increase the fire by degrees, as more and more litharge is formed and absorbed. If the Regulus examined by this assay contain no Silver, you will see it turn wholly into scoria, and at last disappear. When it contains Silver, and the quantity of Lead is much diminished, you will perceive little vivid irises, or beautiful rain-bow colours, shooting swiftly along its surface, and crossing each other in many different directions. At last, when all the Lead is destroyed, the thin dark skin, that is continually protruded by the Lead while it is turning into litharge, and which hitherto covered the Silver, suddenly disappears; and, if at this moment the fire happen not to be strong enough to keep the Silver in fusion, the surface of that metal will at once dart out a dazzling splendour: but, if the fire be strong enough to keep the Silver in fusion, though freed from all mixture of Lead, this change of colour, which is called its fulguration, will not be so perceptible, and the Silver will appear like a bead of fire.

These phenomena shew that the operation is finished. But the cupel must still be left a minute or two under the muffle, and then drawn slowly out with the iron hook towards the door of the furnace. When the Silver is so cooled as to be but moderately red, you may take the cupel from under the muffle with your little tongs, and in the middle of its cavity you will find an exceeding white bead of Silver, the lower part whereof will be unequal, and full of little pits.

OBSERVATIONS.

The Regulus obtained by the former process consists altogether of the Silver contained in the ore, alloyed with the other metals that happened to be mixed therewith in its mineral state, and a good deal of the Lead that was added to precipitate the Silver. The operation of the cupel may be considered as the sequel of that process, being intended only to reduce into a scoria whatever is not Gold or Silver. Lead being of all metals that which vitrifies the most easily, which most promotes the vitrification of the rest, and the only one which, when vitrified, penetrates the cupel, and carries along with it the other metals which it hath vitrified, is consequently the fittest for that purpose. We shall see in its place, that Bismuth hath the same properties with Lead, and may be substituted for it in this operation.

Care must be taken to chuse a cupel of a proper capacity. Indeed it should rather be too big than too little: because the operation is no way prejudiced by an excess in its size; whereas, if it be too small, it will be over-dosed with Lead, and at last the litharge, which destroys every thing, will corrode its cavity, and eat holes through the very body of the vessel. Add, that the ashes, of which the cupel is made, being once glutted with litharge, absorb it afterwards but slowly, and that the quantity of this vitrified litharge, becoming too great to be contained in the substance of the vessel, exsudes through it, and drops on the floor of the muffle, which it corrodes and renders unequal; and moreover solders to it the vessels set thereon. It may be laid down as a general rule for determining the size of a cupel, that it weigh, at least, half as much as the metallic mass to be refined in it.

It is also of the utmost consequence that the cupel be well dried before the metal be put into it. In order to make sure of this point, it must be kept red-hot for a certain time, as is above directed: for though to the sight and to the touch it may appear very dry, it nevertheless obstinately retains a small matter of moisture, sufficient to occasion the loss of some of the metal; which, when it comes to melt, will be thereby spirited up, in the form of little globules, to the very roof of the muffle. The cupels that stand most in need of an intense heat to dry them, are those chiefly in whose composition wood-ashes are employed: for whatever care be taken to lixiviate those ashes before they are used, they will still retain a little alkaline salt; and that, we know, is very greedy of moisture, will not part entirely with it, but by the means of a violent calcination, and presently re-imbibes it when exposed to the air.

A little Phlogiston also may still be left in the ashes of which the cupels are made; and that is another reason for calcining them before they are used. By this means the remaining Phlogiston is dissipated, which might otherwise combine with the litharge during the operation, reduce it, and occasion such a ferment in the matter as to make some of it run over; to these inconveniencies, which any remainder of moisture or Phlogiston may produce, we must add the cracks and flaws, which are very incident to cupels not perfectly freed from both those matters.

It is of no less importance to the success of this operation, that a due degree of heat be kept up. In the process we have described the marks which shew the heat to be neither too strong nor too weak; when it exceeds in either of these respects it may be known by the following signs.

If the fume emitted by the Lead rise like a spout to the roof of the muffle; if the surface of the melted metal be extremely convex, considering the quantity of the mass: if the cupel appear of such a white heat, that the colour communicated thereto by the imbibed scoria cannot be distinguished: all these shew that the heat is too great, and that it ought to be diminished. If, on the contrary, the vapours only hover, as it were, over the surface of the metal; if the melted mass be very flat, considering its quantity; if its ebullition appear but faint; if the scoriæ, that appear like little fiery drops of rain, have but a languid motion; if the scoria gather in heaps, and do not penetrate the cupel; if the metal be covered with it as with a glassy coat; and, lastly, if the cupel look dull; these are proofs that the heat is too weak, and ought to be increased.

The design of this operation being to convert the Lead into litharge, and to give it sufficient time and opportunity to scorify and carry off with it whatever is not Gold or Silver; the fire must be kept up to such a degree that the Lead may easily be turned into litharge, and yet that litharge not be absorbed too hastily by the cupel, but that a small quantity thereof may all along remain, like a ring, round the melted metal.

The fire is to be gradually increased as the operation draws nearer to its end: for, as the proportion of the Lead to the Silver is continually lessening, the metallic mass gradually becomes less fusible; while the Silver defends the Lead mixed with it from the action of the fire, and prevents its being easily converted into litharge.

When the operation is finished, the cupel must still be left under the muffle, till it has imbibed all the litharge, to the end that the bead of Silver may be easily taken out: for, without this precaution, it would stick so fast as not to be removed, but by breaking off part of the cupel along with it. Care must also be taken to let this bead of Silver cool gradually, and be perfectly fixed, before you draw it from under the muffle; for if you expose it at once to the cold air, before it be fixed, it will swell, shoot into sprigs, and even dart out several little grains to a considerable distance, which will be lost.

If the bead appear to have a yellowish tinge, it is a sign that it contains a great deal of Gold, which must be separated from it by the methods to be hereafter shewn.

It is proper to observe, that there is scarce any Lead that does not contain some Silver; too little perhaps to defray the charges necessary to separate it, yet considerable enough to lead us into an error, by mixing with the Silver obtained from an ore, and increasing its weight. And therefore, when the operations above described are applied to the assaying of an ore, in order to know how much Silver it yields, it is previously necessary to examine the Lead to be used, and to ascertain the quantity of Silver it contains, which must be deducted from the total weight of the bead of Silver obtained by purifying it in this manner.

Silver may be separated from its ore, and at the same time refined, by the single operation of the cupel, without any previous scorification with Lead. In order to do this, you must pound the ore; roast it, to dissipate all its volatile parts; mix it with an equal quantity of litharge, if it be refractory; divide it into five or six parcels, wrapping each in a bit of paper; weigh out eight parts of granulated Lead for one of ore, if it be fusible, and from twelve to sixteen, if it be refractory; put one half of the Lead into a very large cupel under the muffle; add thereto one of the little parcels of ore, when the Lead begins to smoke and boil; immediately slacken the fire a little; continue the same degree of heat till you perceive that the litharge formed round the metal, and on its surface, begins to look bright; then raise the fire; add a fresh parcel of ore; continue proceeding in the same manner till you have put in all the ore; then add the remaining half of the granulated Lead, and conduct the succeeding part of the operation in the same manner as that of cupelling.

In this operation it is necessary that the fire be not too strongly urged, and that it be diminished every time you add a fresh parcel of ore; that so the Lead and the litharge may have time to dissolve, scorify, and carry off into the pores of the cupel, all the adventitious matters with which your Silver may be mixed. Notwithstanding this precaution, when the ore is refractory, there often gathers in the cupel a great quantity of scoria, together also with some of the ore that could not be dissolved and scorified. It is with a view to remedy this inconvenience that the second moiety of the Lead is added towards the end, which completes the dissolution and scorification of the whole; so that by means thereof no scoria, or very little, is left in the cupel at the end of the operation.

The operation of the cupel is chiefly used to purify Silver from the alloy of Copper; because this metal, being more fixed and harder to calcine than other metallic substances, is the only one that remains united with Silver and Lead, after roasting and scorification with Lead. It requires no less than sixteen parts of the Lead to destroy it in the cupel, and separate it from Silver. It melts into one mass with the Lead; and the glass produced by these two metals, deprived of their phlogiston, inclines to a brown or a black colour; by which appearance chiefly we know that our Silver was alloyed with Copper.

PROCESS III.

To purify Silver by Nitre.

Granulate the Silver you intend to purify, or reduce it to thin plates; put it into a good crucible; add thereto a fourth part in weight of very dry pulverized Nitre, mixed with half the weight of the Nitre of calcined Wine-lees, and about a sixth part of the same weight of common glass in powder. Cover this crucible with another crucible inverted; which must be of such a size that its mouth may enter a little way into that of the lower one, and have its bottom pierced with a hole of about two lines in diameter. Lute the two crucibles together with clay and Windsor-loam. When the lute is dry, place the crucibles in a melting furnace. Fill the furnace with charcoal, taking care however that the fuel do not rise above the upper crucible.

Kindle the fire, and make your vessels of a middling-red heat. When they are so, take up with the tongs a live-coal, and hold it over the hole of the upper crucible. If you immediately perceive a vivid splendour round the coal, and at the same time hear a gentle hissing noise, it is a sign that the fire is of a proper strength; and it must be kept up at the same degree till this phenomenon cease.

Then increase the fire to the degree requisite to keep pure Silver in fusion; and immediately after take your vessels out of the furnace. You will find the Silver at the bottom of the lower crucible, covered with a mass of Alkaline scoria of a greenish colour. If the metal be not rendered perfectly pure and ductile by this operation, it must be repeated a second time.

OBSERVATIONS.

The purification of Silver by Nitre, as well as the process for refining it on the cupel, is founded on the property which this metal possesses of resisting the force of the strongest fire, and the power of the most active solvents, without losing its phlogiston. The difference between these two operations consists wholly in the substances made use of to procure the scorification of the imperfect metals, or semi-metals, that may be combined with the Silver. In the former this was obtained by Lead, and here it is effected by Nitre. This Salt, as we have shewn, hath the property of calcining and quickly destroying all metallic substances, by consuming their phlogiston, except the perfect metals, Gold and Silver, which alone are able to resist its force. This method may therefore be employed to purify Gold as well as Silver, or indeed both the two mixed together.

In this operation the Nitre is gradually alkalizated, as its Acid is consumed with the phlogiston of the metallic substances. The Alkaline Salt and pounded glass are added, with a view to promote the fusion of the metalline calces, as fast as they are formed, and to fix and retain the Nitre, which, as we shall presently see, is apt to fly off in a certain degree of heat.

The precaution of covering the crucible with another crucible inverted, which hath only a small hole in its bottom, is designed to prevent any of the Silver from being lost in the operation: for when the Nitre comes to be acted on by a certain degree of heat, and especially when it deflagrates with any inflammable matter, part of it flies off, and so rapidly too as to be capable of carrying off with it a good deal of the Silver. The little hole left in the covering crucible is necessary for giving vent to the vapours, which rise during the deflagration of the Nitre, as they would otherwise open themselves a passage by bursting the vessels. After the operation this vent-hole is found beset with many little particles of Silver, which would have been lost if the crucible had not been covered.

If you should observe, during the detonation of the Nitre, that a great many vapours issue through the vent-hole with a considerable hissing noise, even without applying the coal, you must take it for a sign that the fire is too brisk, and accordingly check it; else a great deal of the Nitre will be dissipated, and with it much Silver.

You must observe to take the Silver out of the fire as soon as it is in fusion: for if you neglect this, the Nitre being entirely dissipated or alkalizated, the calces of the metals destroyed by it may possibly recover a little phlogiston, communicated either by the vapours of the charcoal, or by little bits of coal accidentally falling into the crucible; by which means some portion of those metals being reduced will mix again with the Silver, prevent its having the desired degree of purity and ductility, and oblige you to begin the operation afresh.

PROCESS IV.

To dissolve Silver in Aqua Fortis, and thereby separate it from every other metalline substance. The Purification of Aqua Fortis. Silver precipitated by Copper.

The Silver you intend to dissolve being beaten into thin plates, put it into a glass cucurbit; pour on it twice its weight of good precipitated aqua fortis; cover the cucurbit with a piece of paper, and set it on a sand-bath moderately heated. The aqua fortis will begin to dissolve the Silver as soon as it comes to be a little warm. Red vapours will rise; and from the upper surfaces of the Silver there will seem to issue streams of little bubbles, ascending to the top of the liquor, between which and the Silver they will form, as it were, a number of fine chains: this is a sign that the dissolution proceeds duly, and that the degree of heat is such as it ought to be. If the liquor appear to boil and be agitated, a great many red vapours rising at the same time, it is a sign that the heat is too great, and should be lessened till it be reduced to the proper degree indicated above: having obtained that, keep it equally up till no more bubbles or red vapours appear.

If your Silver be alloyed with Gold, the Gold will be found, when the dissolution is finished, at the bottom of the vessel in the form of a powder. This solution must now be decanted while it is yet warm; on the powder pour half as much fresh aqua fortis as before, and make it boil; again decant this second aqua fortis, and repeat the same a third time; then with fair water wash the remaining powder well: it will be of a brown colour inclining to red. In the observations we shall show how the Silver is to be separated from the aqua fortis.

OBSERVATIONS.

All the processes on Silver already delivered, whether for extracting it from its ores, or for refining it, either by the Cupel or by Nitre, are applicable to Gold also. And if Silver be alloyed with Gold before it undergo those several operations, it will still remain alloyed therewith after them, in the same manner, and in the same quantity; because both metals bear them equally. All therefore that can be expected from those several assays, is the separation of every thing that is neither Silver nor Gold from these two metals. But in order to separate these two from each other, recourse must be had either to the process laid down under the head of Gold, or to that here described, which is the most commodious, the most usual, and known by the names of Quartation and the Parting Assay.

Aqua fortis is the true solvent of Silver, and is utterly incapable of dissolving the least atom of Gold. If therefore a mass consisting of Gold and Silver be exposed to the action of aqua fortis, that Acid will dissolve the Silver contained in the compound, without touching the Gold, and the two metals will be separated from each other. This method of parting them is just the reverse of that described before under the head of Gold, which is effected by the means of aqua regis.

To the success of this separation, by means of aqua fortis, several conditions are essentially necessary. The first is, that the Gold and Silver be in due proportion to each other; that is, there must be at least twice as much Silver as Gold in the metalline mass, otherwise the aqua fortis will not be able to dissolve it, for the reason formerly given. If therefore the mass contain too little Silver, it must either be melted down again, and a proper quantity of Silver added; or else, if the Gold be in a sufficient proportion to the Silver, they may be parted by means of aqua regis.

Secondly, it is necessary that the aqua fortis employed in this operation be absolutely pure, and free from any taint of the Vitriolic or Marine Acid: for, if it be adulterated with the Vitriolic Acid, the Silver will precipitate as fast as it dissolves, and so the precipitated Silver will again mix with the Gold. If the aqua fortis contain any of the Marine Acid, the Silver will be precipitated in that case also; and this inconvenience will be attended with another, namely, that the menstruum, being partly an aqua regis, will dissolve some of the Gold. You must therefore be very sure that your aqua fortis is pure, before you set about the operation. In order to discover its quality, you must try it by dissolving, in a small portion thereof, as much Silver as it will take up: if the aqua fortis grow opaque and milky as it dissolves the Silver, it is a sign it contains some foreign Acid, from which it must be purified.

In order to effect this, let the portion of aqua fortis used for the above trial stand to settle: the white milky part will gradually fall to the bottom of the vessel. When it is all fallen, gently decant the clear liquor, and pour a few drops of this decanted solution of Silver into the aqua fortis which you want to purify. It will instantly become milky. Let the white particles precipitate as before, and then add a few more drops of your solution of Silver. If the aqua fortis still become milky, let it precipitate again, and repeat this till you find that a drop of your solution of Silver, let fall into this aqua fortis, does not make it in the least turbid. Then filter it through brown paper, and you will have an aqua fortis perfectly fit for the Parting Assay.

The white particles that appear and settle to the bottom, on dissolving silver in an aqua fortis adulterated with a mixture of some foreign Acid, are no other than that very Silver, which is no sooner dissolved by the Nitrous Acid than it deserts that solvent to unite with the Vitriolic or Marine Acid, wherewith it has a greater affinity, and falls to the bottom with them. And this happens as long as there remains in the aqua fortis a single atom of either of those two Acids.

When therefore your aqua fortis hath dissolved as much Silver as it is capable of taking up, and when all the white particles formed during the dissolution are settled to the bottom, you may be assured that the portion which remains clear and limpid is a solution of Silver in an exceeding pure aqua fortis. But if the solution of Silver thus depurated be mixed with an aqua fortis adulterated with the Vitriolic or Marine Acid, a like precipitation will immediately ensue, for the reasons above given, till the very last particle of the heterogeneous Acid contained in the aqua fortis be precipitated.

Aqua fortis purified by this method contains no extraneous substance whatever, except a small portion of Silver; so that it is very fit for the parting process. But if it be intended for other chymical purposes, it must be rectified in a glass retort with a moderate heat, in order to separate it from the small portion of Silver it contains, which will remain at the bottom of the retort.

The third condition necessary to the success of this operation is, that your aqua fortis be neither too aqueous, nor too highly concentrated. If too weak, it will not act upon the Silver: and the consequence will be the same if it be too strong. Both these inconveniencies are easily remedied: for in the former case part of the superfluous phlegm may be drawn off by distillation; or a sufficient quantity of much stronger aqua fortis may be mixed with that which is too weak: and, in the latter case, very pure rain water, or a weaker aqua fortis, may be mixed with that which is too strong.

You may satisfy yourself whether or no your aqua fortis hath the requisite degree of strength, by dissolving therein a thin plate consisting of one part Gold and two or three parts Silver; which plate must be rolled up in form of a paper coffin. If, when all the Silver contained in the plate is dissolved, the Gold remains in the form of the coffin, it is a sign that your solvent has a due degree of strength. If, on the contrary, the Gold be reduced to a powder, it is a proof that your aqua fortis is too strong, and ought to be weakened.

The Gold remaining after the dissolution of the Silver must be melted in a crucible with Nitre and Borax, as hath already been said under the process for parting Gold and Silver by means of aqua regis. As to the Silver which remains dissolved in the aqua fortis, there are several ways to recover it.

The most usual is to precipitate it by the interposition of Copper, which hath a greater affinity than Silver with the Nitrous Acid. For this purpose the solution is weakened by adding twice or thrice as much very pure rain water. The cucurbit containing the solution is set on a sand-bath gently heated, and very clean plates of copper put into it. The surfaces of these plates are soon covered with little white scales, which gradually fall to the bottom of the vessel, as they come to be collected in quantities. It is even proper to strike the cucurbit gently now and then, in order to shake the scales of Silver from the copper plates, and so make room for a new crop.

See the Table of Affinities, Column IV.

The aqua fortis parts with the Silver by degrees only, as it dissolves the Copper; and therefore the liquor gradually acquires a blueish green colour as the precipitation advances. This precipitation of the Silver is to be continued as long as any remains dissolved in the aqua fortis: you may be sure that your liquor contains no more Silver, if the surface of a fresh plate of Copper laid therein remain clean and free from ash-coloured or greyish particles: or if one drop of a solution of Sea-salt let fall into it produce no white or milky cloud.

The precipitation being finished, the liquor is to be gently poured off from the precipitated Silver, which must be rinsed in several waters, and even made to boil therewith, in order to free it wholly from the dissolved Copper. The Silver thus well washed must be thoroughly dried, mixed with a fourth part of its weight of a flux compounded of equal parts of Nitre and calcined Borax, and then melted in a crucible. On this occasion care must be taken to raise the fire gently and gradually, till the Silver be brought to fusion.

With what accuracy soever the precipitated Silver be washed, in order to free it from the solution of Copper, yet the Silver will always be found alloyed with a small portion of the Copper: but then this Copper is easily destroyed by the Nitre, with which the Silver is afterwards melted; so that the latter metal remains perfectly pure after the operation.

Though the Silver be not previously cupelled, but be alloyed with other metallic substances at the time it is thus dissolved, yet the dissolving, precipitating, and fusing it with Nitre, would be sufficient to separate it accurately from them all, and refine it to a degree of purity equal to that obtained by the cupel.

The Copper that remains dissolved in the aqua fortis, after the precipitation of the Silver, may in like manner be precipitated by Iron, and, as it retains a small portion of Silver, ought not to be neglected when these operations are performed on considerable quantities.

In the two next processes we shall shew two other methods of separating Silver from aqua fortis.

PROCESS V.

To separate Silver from the Nitrous Acid by Distillation. Crystals of Silver. The Infernal Stone.

Into a large, low, glass body put the solution of Silver, from which you intend to separate the Silver by distillation. To this body fit a tubulated head provided with its stopple. Set this alembic in a sand-bath, so that the body may be almost covered with sand: apply a receiver, and distil with a moderate heat, so that the drops may succeed each other at the distance of some seconds. If the receiver grow very hot, check the fire. When red vapours begin to appear, pour into the alembic, through the hole in its head, a fresh quantity of your solution of Silver, first made very hot. Continue distilling in this manner, and repeating the addition of fresh liquor, till all your solution be put into the alembic. When you have no more fresh solution to put in, and when, the phlegm being all come over, red vapours begin again to appear, convey into the alembic half a dram or a dram of tallow, and distil to dryness; which being done, increase your fire so as to make the vessel containing the sand-bath red-hot. In the alembic you will find a calx of Silver, which must be melted in a crucible with some soap and calcined wine-lees.

OBSERVATIONS.

A low cucurbit is recommended for this operation, to the intent that the particles of the Nitrous Acid, which are ponderous, may the more easily be carried up and pass over into the receiver. For the same reason the cucurbit is directed to be almost wholly covered with sand, lest otherwise the acid vapours should be condensed about that part of the cucurbit, which, being out of the sand, would be much cooler than that which is encompassed therewith, and from thence should fall back again to the bottom; by which means the distillation would certainly be retarded, and the vessel probably be broken.

Notwithstanding these precautions the vessels are liable to break in such distillations; especially when they contain a great deal of liquor. With a view, therefore, to prevent this accident, we ordered that the whole quantity of the solution of Silver to be distilled should not be put at once into the alembic. The little bit of tallow, added towards the end of the operation, is intended to hinder the metal from adhering closely to the vessel, as it would otherwise do, when all the moisture is dissipated.

The Soap and Fixed Alkali mixed with the Silver to flux it, after its separation from the aqua fortis in this way, serve to absorb such of the most fixed particles of the Acid as may still remain united with the metal.

If the distillation be stopped when part of the phlegm is drawn off, and the liquor be then suffered to cool, many crystals will shoot therein, which are a Neutral Salt constituted of the Nitrous Acid and Silver. If the distillation be carried further, and stopped when near its conclusion, the liquor being then suffered to cool will wholly coagulate into a blackish mass called the Infernal Stone.

This way of separating Silver from its solvent is attended with the advantage of saving all the aqua fortis, which is excellent, and fit to be employed in other operations.

PROCESS VI.

To separate Silver from the Nitrous Acid by Precipitation. Luna Cornea. Luna Cornea reduced.

Into your solution of Silver pour about a fourth part in weight of Spirit of Salt, solution of Sea-salt, or solution of Sal Ammoniac. The liquor will instantly become turbid and milky. Add twice or thrice its weight of fair water, and let it stand some hours to settle. It will deposite a white powder. Decant the clear liquor, and on the precipitate pour fresh aqua fortis, or Spirit of Salt, and warm the whole on a sand-bath with a gentle heat for some time. Pour off this second liquor, and boil your precipitate in pure water, shifting it several times, till the precipitate and the water be both quite insipid. Filter the whole, and dry the precipitate, which will be a Luna Cornea, and must be reduced in the following manner.

Smear the inside of a good crucible well with soap. Put your Luna Cornea into it; cover it with half its weight of Salt of Tartar, thoroughly dried and pulverized; press the whole hard down; pour thereon as much oil, or melted tallow, as the powder is capable of imbibing; set the crucible thus charged, and close covered, in a melting furnace, and, for the first quarter of an hour, make no more fire than is necessary to make the crucible moderately red: after that raise it so as to melt the Silver and the Salt, throwing into the crucible from time to time little bits of tallow. When it ceases to smoke, let the whole cool; or pour it into a hollow iron cone, warmed and tallowed.

OBSERVATIONS.

The process here delivered furnishes us with the means of procuring Silver in a degree of purity which is not to be obtained by any other method of treating it whatever. That which is refined on the cupel always retains a small portion of Copper, from which it cannot possibly be separated in that way: but if it be dissolved in aqua fortis, and precipitated thence in a Luna Cornea by the Marine Acid, the precipitate will be an absolutely pure Silver, unalloyed with that small portion of Copper which is retained on the cupel. The reason of this effect is, that the Copper remains as perfectly dissolved in Spirit of Salt and in aqua regia as in aqua fortis: so that when the Silver, and the Copper with which it is alloyed, are dissolved together in the Nitrous Acid, if the Acid of Sea-salt be mixed with the solution, part of this latter Acid unites with the Silver, and therewith forms a new compound, which not being soluble in the liquor, falls to the bottom. The other part of the Acid mixing with the Nitrous, forms an aqua regis, in which the Copper remains dissolved, without separating from it.

Fresh Acid is poured on the precipitated calx of Silver, in order to complete the solution of the small portion of Copper that may have escaped the action of the first solvent. It is indifferent whether the Spirit of Salt or the Spirit of Nitre be employed for this purpose, because they both dissolve Copper alike, and because Silver precipitated by Spirit of Salt is not soluble in either.

After this it is necessary to wash the precipitate well with pure water, in order to free it entirely from the particles of aqua fortis adhering to the Silver; because they may possibly contain something of Copper, which would mix with the Silver in melting, and taint its purity.

If this precipitate of Silver be exposed to the fire, unmixed with any other substance, it melts as soon as it begins to be red; and, if the fire be increased, part thereof will be dissipated in vapours, and the rest will make its way through the crucible. But being poured out as soon as melted, it coagulates into a cake of a purplish red colour, semi-transparent, ponderous, and in some degree pliable, especially if it be very thin. It bears some resemblance to horn, which hath occasioned it to be called Luna Cornea.

As Luna Cornea is not soluble in water, recourse must be had to fusion, in order to reduce it, by separating from the Silver those acids which give it the above-mentioned properties. Fixed Alkalis and fatty matters are very fit to produce that separation.

We directed that the inside of the crucible, in which the reduction is to be made, should be carefully smeared with soap, and that the Luna Cornea should be quite covered with a Fixed Alkali and fat, to the end that when the heat is strong enough to dissipate it in vapours, or to attenuate it so as to render it capable of penetrating the crucible, it may be forced to pass through matters qualified to absorb its Acid, and reduce it.

Luna Cornea may also be reduced by being melted with such metalline substances as have a greater affinity than Silver with the Acids wherewith it is impregnated. Of this kind are Tin, Lead, Regulus of Antimony: but the Luna Cornea rushes so impetuously into conjunction with those metalline substances, that a vast many vapours arise, and carry off with them part of the Silver: if therefore you chuse to effect the reduction by the interposition of such metalline substances, you must employ a retort instead of a crucible.

But this method is attended with another inconvenience; which is, that some part of those metalline substances may unite with the Silver, and adulterate it: for which reason it is best to keep to the method first proposed.

PROCESS VII.

To dissolve Silver, and separate it from Gold, by Cementation.

Mix thoroughly together fine brick-dust four parts, Vitriol calcined to redness one part, and Sea-salt or Nitre one part. Moisten this powder with a little water. With this cement cover the bottom of a crucible half an inch thick; on this first bed lay a thin plate of the mass of Gold and Silver you intend to cement, and which you must previously take care to beat into such thin plates. Cover this plate with a second layer of cement, of the same thickness as the former; on this second bed lay another plate of your metal; cover it in like manner with cement; and so proceed till the crucible be filled to within half an inch of its brim. Fill up the remaining space with cement, and close the crucible with a cover, luted with a paste made of Windsor-loam and water: set your crucible thus charged in a furnace, whose fire-place is deep enough to let it be entirely surrounded with coals, quite up to its mouth. Light some coals in the furnace, taking care not to make the fire very brisk at first; increase it by degrees, but only so far as to make the crucible moderately red; keep up the fire in this degree for eighteen or twenty hours: then let the fire go out; open the crucible when it is cold, and separate the cement from your plates of Gold. Boil the Gold repeatedly in fair water, till the water come off quite insipid.

OBSERVATIONS.

It cannot but seem strange, that, after having so often declared the Acid of Sea-salt to be incapable of dissolving Silver, we should direct either Nitre or Sea-salt indifferently to be employed in composing a cement, which is to produce an Acid capable of eating out all the Silver mixed with Gold. It is easy to conceive how the Nitrous Acid extricated from its basis by means of the Vitriolic Acid may produce this effect: but if Sea-salt instead of Nitre be made an ingredient in the cement, its Acid, though set at liberty in the same manner by the Vitriolic Acid, must at first sight appear unable to answer the end.

In order to remove this difficulty, we must here observe, that there are two very essential differences between the Marine Acid collected in a liquor, as it is when distilled in the usual manner, and the same Acid separated from its basis in a crucible, as it is in cementation.

The first of these two differences is, that the Acid being reduced into vapours when it acts on the Silver in cementation, its activity is thereby greatly increased: the second is, that in the crucible it sustains a vastly greater degree of heat than it can ever bear when it is in the form of a liquor. For, after it is once distilled and separated from its basis, it cannot sustain any extraordinary degree of heat without being volatilized and entirely dissipated: whereas, while it continues united with its basis, it is much more fixed, and cannot be separated but by a very intense heat. Consequently, if it meet with any body to dissolve, at the very instant of its separation from its basis, while it is actuated by a much fiercer heat than can ever be applied to it on any other occasion, it must operate upon that body with so much the more efficacy: and thus it comes to pass, that in cementation it has the power of dissolving Silver, which it would be incapable of touching if it were not so circumstanced.

But herein Gold differs from Silver: for, whatever force the Nitrous or the Marine Acid may exert, when extricated from their bases in the cementing crucible, this metal obstinately refuses to yield to either of those Acids separately, and can never be dissolved by them, unless both be united together.

Our cementation, therefore, is actually a parting process in the dry way. The Silver is dissolved, and the Gold remains unaltered. Nay, as the action of the Acids is much stronger when they are applied this way, than when they are used for dissolution in the moist way, the Nitrous Acid, which in the common parting process will not dissolve Silver unless its weight be double that of the Gold, is able in cementation to dissolve a very small quantity of Silver diffused through a large quantity of Gold.

It sometimes happens, that after the operation the cement proves extremely hard, so that it is very troublesome to separate it entirely from the Gold. In this case it must be softened by moistening it with hot water. This hardness which the cement acquires is occasioned by the fusion of the Salts, which is the effect of too strong a heat. It was in order to prevent this, and that a due degree of heat might be applied, without the danger of melting the salts, that we directed the cement to be mixed with a considerable quantity of earthy matter incapable of fusion, such as brick-dust. A greater inconvenience will ensue, if the fire be made so strong as to melt the Gold: for then it will partly commix again with the other metalline substances dissolved by the cement, and consequently will not be purified.

The crucible is covered, and its cover luted on, to prevent the acid vapours from being too soon dissipated, and to force them to circulate the longer in the crucible. However, it is necessary that those vapours should find a vent at last, otherwise they would burst the vessel: and for this reason we directed the crucible to be luted only with Windsor-loam, which does not grow very hard by the action of fire, and so is capable of yielding and giving passage to the vapours, when a certain quantity of them is collected in the crucible, and they begin to struggle for an escape on every side.

When the operation is finished, the Silver dissolved by the Acid of the cement is partly distributed through the cement, and partly in the Gold itself, which is impregnated therewith. For this reason the Gold must be washed several times in boiling water, till the water become absolutely insipid: for, if the Gold be melted without this precaution, it will mix again with the Silver: the cement also may be washed in the same manner to recover the Silver it contains.

Though this cementation be, properly speaking, a purification of Gold, yet we have placed it among the processes on Silver, because it is the Silver that is dissolved on this occasion, and because this is a particular way of dissolving that metal. Moreover, most of the processes hitherto delivered, either on Gold or Silver, are equally applicable to both these metals.

If the Gold do not appear quite pure after the cementation, the process must be repeated.

There are several ways to know the fineness of Gold, the quantity of Silver with which it is alloyed, and the proportion in which these two metals are mixed in a mass purified by the cupel.

One of the simplest is the trial by the Touch-stone; which indeed is hardly any more than judging by the eye only, from the colour of the compound metal, what proportion of Gold and Silver it contains.

The Touch-stone is a sort of black marble, whose surface ought to be half polished. If the metalline mass which you want to try be rubbed on this stone, it leaves thereon a thin coat of metal, the colour of which may be easily observed. Such as are accustomed to see and handle Gold and Silver can at once judge very nearly from this sample in what proportion the two metals are combined: but, for greater accuracy, those who are in the way of having frequent occasion for this trial are provided with a sufficient number of small bars or needles, of which one is pure Gold, another pure Silver, and all the rest consist of these two metals mixed together in different proportions, varied by carats, or even by fractions of carats, if greater exactness be required.

The fineness of each needle being marked on it, that needle whose colour seems to come nearest the colour of the metalline streak on the Touch-stone, is rubbed on the stone by the side of that streak. This needle likewise leaves a mark; and if there appear to be no difference between the two metalline streaks, the metalline mass is judged to be of the same fineness as the needle thus compared with it. If the eye discovers a sensible difference, another needle is sought for whose colour may come nearer to that of the metal to be tried. But though a man be ever so well versed in judging thus of the fineness of Gold by the eye only, he can never be perfectly and accurately sure of it by this means alone. If such certainty be required, recourse must be had to the parting assay; and yet when you have gone through it, there always remains a small quantity of the metal, which should have been dissolved, and yet escaped the action of the solvent. For example, if you make use of aqua regis, the Silver that remains after the operation still contains a little Gold; and, if you make use of aqua fortis, the Gold that remains after the operation still contains a little Silver. And therefore if you resolve to carry the separation of these two metals still further by solvents, it will be necessary, after you have gone through one parting process, to perform a second the contrary way. For example, if you begin with aqua fortis, then, after it has dissolved all the Silver in the metalline mass that it is capable of taking up, dissolve the remaining Gold in aqua regis: by which means you will separate the small portion of Silver left in it by the aqua fortis. The contrary is to be done if you made use of aqua regis first.

CHAP. III.

Of COPPER.

PROCESS I.

To separate Copper from its Ore.

Beat your Copper ore to a fine powder, having first freed it as accurately as possible, by washing and roasting, from all stony, earthy, sulphureous, and arsenical parts. Mix your ore thus pulverized with thrice its weight of the black flux; put the mixture into a crucible; cover it with common salt to the thickness of half an inch, and press the whole down with your finger. With all this the crucible must be but half full. Set it in a melting furnace; kindle the fire by degrees, and raise it insensibly till you hear the Sea-salt crackle. When the decrepitation is over, make the crucible moderately red-hot for half a quarter of an hour. Then give a considerable degree of heat, exciting the fire with a pair of good perpetual bellows, so that the crucible may become very red-hot, and be perfectly ignited. Keep the fire up to this degree for about a quarter of an hour; then take out the crucible, and with a hammer strike a few blows on the floor whereon you set it. Break it when cold. If the operation hath been rightly and successfully performed, you will find at the bottom of the vessel a hard Regulus, of a bright yellow colour, and semi-malleable; and over it a scoria of a yellowish brown colour, hard and shining, from which you may separate the Regulus with a hammer.

OBSERVATIONS.

Copper in the ore is often blended with several other metallic substances, and with volatile minerals, such as Sulphur and Arsenic. Copper ores also frequently participate of the nature of the pyrites, containing a martial and an unmetallic earth, both of which are entirely refractory, and hinder the ore from melting. In this case you must add equal parts of a very fusile glass, a little borax, and four parts of the black flux, to facilitate the fusion. The black flux is moreover necessary to furnish the Copper with the Phlogiston it wants, or restore so much thereof as it may lose in melting. For the same reason, when any ore, but that of Gold or Silver, is to be smelted, it is a general rule to add some black flux, or other matter abounding with Phlogiston.

The Regulus produced by this operation is not malleable, because it is not pure Copper, but a mixture of Copper with all the other metallic substances that were in the ore; except such as were separated from it by roasting, of which it contains but little.

According to the nature of the metallic matters that remain combined with the Copper after this fusion, the colour of the Regulus is either like that of pure Copper, or a little more whitish: it is also frequently blackish, which has procured it the name of Black Copper. In this state, and even in general, it is usual enough to call this Regulus by the name of Black Copper, when alloyed with other metallic substances that render it unmalleable, whatever its colour be.

Hence it appears that there may be several different sorts of Black Copper. Iron, Lead, Tin, Bismuth, and the reguline part of Antimony, are almost always combined with the ores of Copper, in a multitude of different proportions; and all these substances, being reduced by the black flux in the operation, mix and precipitate with the Copper. If the ore contain any Gold or Silver, as is pretty often the case, these two metals also are confounded with the rest in the precipitation, and become part of the Black Copper.

Pyritose, sulphureous, and arsenical Copper ores may be fused, in order to get rid of the grosser heterogeneous parts, without previously roasting them: but in this case no alkaline flux must be mixed with the ore; because the Alkali in combination with the Sulphur would produce a Liver of Sulphur, and so dissolve the metalline part; by which means all would be confounded together, and no Regulus, or very little, be precipitated. On this occasion therefore nothing must be added to promote the fusion, but some tender fusile glass, together with a small quantity of borax.

This first fusion may also be performed amidst the coals, by casting the ore upon them in the furnace, without using a crucible; and then an earthen vessel, thoroughly heated, or even made red-hot, must be placed under the grate of the fire-place, to receive the metal as it runs from the ore.

The Regulus obtained by this means is much more impure and brittle than Black Copper, because it contains moreover a large quantity of Sulphur and Arsenic; as these volatile substances have not time to evaporate during the short space requisite to melt the ore, and as they cannot be carried off by the action of the fire after the ore is once melted, whatever time be allowed for that purpose. However, some part thereof is dissipated; and the Iron which is in pyritose ores, having a much greater affinity than Copper, and indeed than any other metallic substance, with Sulphur and Arsenic, absorbs another part thereof, and separates it from the Regulus.

This Regulus, it is plain, still contains all the same parts that were in the ore, but in different proportions; there being more Copper, combined with less Sulphur, Arsenic, and unmetallic earth, which have been either dissipated or turned to slag. Therefore, if you would make it like Black Copper, you must pound it, roast it over and over, to free it from its Sulphur and Arsenic, and then melt it with the black flux.

If this Regulus contain much Iron, it will be adviseable to melt it once or twice more, before all the Sulphur and Arsenic are separated from it by roasting; for as the Iron, by uniting with these volatile substances, separates them from the Copper, with which they have not so great an affinity; so also the Sulphur and Arsenic, by uniting with the Iron, help in their turn to separate it from the Copper.

PROCESS II.

To purify Black Copper, and render it malleable.

Break into small bits the Black Copper you intend to purify; mix therewith a third part in weight of granulated Lead, and put the whole into a cupel set under the muffle in a cupelling furnace, and previously heated quite red. As soon as the metals are in the cupel raise the fire considerably, making use, if it be needful, of a pair of perpetual bellows, to melt the Copper speedily. When it is thoroughly melted, lower the fire a little, and continue it just high enough to keep the metalline mass in perfect fusion. The melted matter will then boil, and throw up some scoriæ, which will be absorbed by the cupel.

When most of the Lead is consumed, raise the fire again, till the face of the Copper become bright and shining, thereby shewing that all its alloy is separated. As soon as your Copper comes to this state, cover it with charcoal-dust conveyed into the cupel with an iron ladle: then take the cupel out of the furnace and let it cool.

OBSERVATIONS.

Of all the metals, next to Gold and Silver, Copper bears fusion the longest without losing its phlogiston; and on this property is founded the process here delivered for purifying it.

It is necessary the Copper should melt as soon as it is in the cupel, because its nature is to calcine much more easily and much sooner, when it is only red-hot, than when it is in fusion. For this reason the fire is to be considerably raised, immediately on putting the Copper under the muffle, that it may melt as soon as possible. Yet too violent a degree of fire must not be applied to it: for when it is exposed to such a degree of heat only as is but just necessary to keep it in fusion, it is then in the most favourable condition for losing as little as may be of its phlogiston; and if the heat be stronger, a greater quantity thereof will be calcined. As soon therefore as it flows it is proper to weaken the fire, and reduce it to the degree just requisite to keep up the fusion.

The Lead added on this occasion is intended to facilitate and expedite the scorification of the metallic substances combined with the Copper. So that the event is here nearly the same as when Gold or Silver is refined on the cupel. The only difference between this refining of Copper, and that of the perfect metals, is that the latter as hath been shewn, absolutely resist the force of fire and the action of Lead, without suffering the least alteration; whereas a good deal of Copper is calcined and destroyed, when it is purified in this manner on the cupel. Indeed it would be wholly destroyed, if a greater quantity of Lead were added, or if it were left too long in the furnace. It is with a view to save as much of it as possible that we order it to be covered with charcoal-dust as soon as the scorification is finished.

The Lead serves moreover to free the Copper expeditiously from the Iron with which it may be alloyed. Iron and Lead are incapable of contracting any union together: so that as fast as the Lead unites with the Copper, it separates the Iron, and excludes it out of the mixture. For the same reason if Iron were combined in a large proportion with Copper, it would prevent the Lead from entering into the composition. Now, as it is necessary to give the more heat, and to keep the Copper to be incorporated with Lead the longer in fusion, as that Copper is alloyed with a greater proportion of Iron, some black flux must be added on this occasion, to prevent the Copper and the Lead from being calcined before their association can be effected.

Copper purified in the manner here directed is beautiful and malleable. It is now alloyed with no other metalline substance but Gold or Silver, if there were any in the mixed mass. If you desire to extract this Gold or Silver, recourse must be had to the operation of the cupel. The process here given for purifying Copper is not used in large works, because it would be much too chargeable. In order to purify their Black Copper, and render it malleable, the smelters content themselves with roasting it, and melting it repeatedly, that the metallic substances, which are not so fixed as Copper, may be dissipated by sublimation, and the rest scorified by fusion.

PROCESS III.

To deprive Copper of its Phlogiston by calcination.

Put your Copper in filings into a test, and set it under the muffle of a cupelling furnace; light the fire, and keep up such a degree of heat as may make the whole quite red, but not enough to melt the Copper. The surface of the Copper will gradually lose its metalline splendour, and put on the appearance of a reddish earth. From time to time stir the filings with a little rod of copper or iron, and leave your metal exposed to the same degree of fire till it be entirely calcined.

OBSERVATIONS.

In our observations on the preceding process we took notice that Copper, in fusion, calcines more slowly, and less easily, than when it is exposed to a degree of fire barely sufficient to keep it red-hot, without melting it; and therefore, the design here being to calcine it, we have directed that degree of heat only to be applied.

The cupelling furnace is the fittest for this operation, because the muffle is capable of receiving such a flat vessel as ought to be used on this occasion, and communicating to it a great deal of heat; while, at the same time, it prevents the falling in of any coals, which, by furnishing the Copper with fresh phlogiston, would greatly prejudice and protract the operation.

As Copper calcines with great difficulty, this operation is extremely tedious: nay, though Copper hath stood thus exposed to the fire for several days and nights, and seems perfectly calcined, yet it frequently happens that, when you try afterwards to melt it, some of it resumes the form of Copper: a proof that all the Copper had not lost its phlogiston. Copper is much more expeditiously deprived of its phlogiston by calcining it in a crucible with Nitre.

The calx of Copper perfectly calcined is with great difficulty brought to fusion: yet, in the focus of a large burning-glass, it melts and turns to a reddish and almost opaque glass.

By the process here delivered, you may likewise calcine all other metalline substances, which do not melt till they are thoroughly red-hot. As to those which melt before they grow red, they are easily enough calcined, even while they are in fusion.

PROCESS IV.

To resuscitate the Calx of Copper, and reduce it to Copper, by restoring its Phlogiston.

Mix the Calx of Copper with thrice as much of the black flux; put the mixture into a good crucible, so as to fill two thirds thereof, and over it put a layer of Sea-salt a finger thick. Cover the crucible, and set it in a melting furnace; heat it gradually, and keep it moderately red till the decrepitation of the Sea-salt be over. Then raise the fire considerably by means of a good pair of perpetual bellows; satisfy yourself that the matter is in perfect fusion, by dipping into the crucible an iron wire; continue the fire in this degree for half a quarter of an hour. When the crucible is cold, you will find at its bottom a button of very fine Copper, which will easily separate from the saline scoria at top.

OBSERVATIONS.

What hath been said before on the smelting of Copper ores may be applied to this process, as being the very same. The observations there added should therefore be consulted on this occasion.

PROCESS V.

To dissolve Copper in the Mineral Acids.

On a sand-bath, in a very gentle heat, set a matrass containing some Copper filings; pour on them twice their weight of Oil of Vitriol. That Acid will presently attack the Copper. Vapours will rise, and issue out of the neck of the matrass. A vast number of bubbles will ascend from the surface of the metal to the top of the liquor, and the liquor will acquire a beautiful blue colour. When the Copper is dissolved, put in a little and a little more, till you perceive the Acid no longer acts upon it. Then decant the liquor, and let it stand quiet in a cool place. In a short time great numbers of beautiful blue crystals will shoot in it. These crystals are called Vitriol of Copper, or Blue Vitriol. They dissolve easily in water.

OBSERVATIONS.

The Vitriolic Acid perfectly dissolves Copper, which is also soluble in all the Acids, and even in many other menstruums.

This Acid may be separated from the Copper which it hath dissolved by distillation only: but the operation requires a fire of the utmost violence. The Copper remaining after it must be fused with the black flux, to make it appear in its natural form; not only because it still retains a portion of the Acid, but also because it hath lost part of its phlogiston by being dissolved therein. The black flux is very well adapted both to absorb the Acid that remains united with the Copper, and to restore the phlogiston which the metal hath lost.

The most usual method of separating Copper from the Vitriolic Acid is by presenting to that Acid a metal with which it hath a greater affinity than with Copper. Iron being so qualified is consequently very fit to bring about this separation. When therefore plates of Iron well cleaned are laid in a solution of Blue Vitriol, the Acid soon begins to act upon them, and by degrees, as it dissolves them, deposites on their surfaces a quantity of Copper in proportion to the quantity of Iron it takes up. The Copper thus precipitated hath the appearance of small leaves or scales, exceeding thin, and of a beautiful copper-colour. Care must be taken to shake the Iron-plates now and then, to make the scales of Copper fall off, which will otherwise cover them entirely, hinder the Vitriolic Acid from attacking the Iron, and so put a stop to the precipitation of the remaining Copper.

When these scales of Copper cease to settle on the clean Iron plates, you may be sure all the Copper that was in the liquor is precipitated, and that this liquor, which was a solution of Copper before the precipitation, is a solution of Iron after it. So that here two operations are performed at one and the same time; to wit, the precipitation of the Copper, and the dissolution of the Iron.

The Copper thus precipitated requires only to be separated from the liquor by filtration, and melted with a little black flux, to become very fine malleable Copper.

The Copper may also be precipitated out of a solution of Blue Vitriol by the interposition of a Fixed Alkali. This precipitate is of a greenish blue colour, and requires a much greater quantity of the black flux to reduce it.

Copper dissolves in the Nitrous Acid, in the Marine Acid, and in Aqua regis; from all of which it may be separated by the same methods as are here ordered with regard to the Vitriolic Acid.

CHAP. IV.

Of IRON.

PROCESS I.

To separate Iron from its Ore.

Pound into a coarse powder the martial stones or earths out of which you design to extract the Iron: roast this powder in a test under the muffle for some minutes, and let your fire be brisk. Then let it cool, beat it very fine, and roast it a second time, keeping it under the muffle till it emit no more smell.

Then mix with this powder a flux composed of three parts of Nitre fixed with Tartar, one part of fusile glass, and half a part of Borax and charcoal-dust. The dose of this reducing flux must be thrice the weight of the ore.

Put this mixture into a good crucible; cover it with about half a finger thick of Sea-salt; over the crucible put its cover, and lute it on with Windsor-loam made into a paste with water. Having thus prepared your crucible, set it in a melting furnace, which you must fill up with charcoal. Light the fire, and let it kindle by gentle degrees, till the crucible become red-hot. When the decrepitation of the Sea-salt is over, raise your fire to the highest by the blast of a pair of perpetual bellows, or rather several. Keep up this intense degree of heat for three quarters of an hour, or an whole hour, taking care that during all this time the furnace be kept constantly filling up with fresh coals as the former consume. Then take your crucible out of the furnace; strike the pavement on which you set it several times with a hammer, and let it stand to cool: break it, and you will find therein a Regulus of Iron covered with slag.

OBSERVATIONS.

Iron ore, like all others, requires roasting, to separate from it, as much as possible, the volatile minerals, Sulphur and Arsenic, which being mixed with the Iron would render it unmalleable. Indeed it is so much the more necessary to roast these ores, as Iron is, of all metallic substances, that which has the greatest affinity with those volatile minerals; on which account no metallic substance whatever is capable of separating it from them by fusion and precipitation.

Fixed Alkalis, it is true, have a greater affinity than Iron with Sulphur; but then the composition which a Fixed Alkali forms with Sulphur is capable of dissolving all metals. Consequently, if you do not dissipate the Sulphur by roasting, but attempt to separate it from the Iron by melting the ore with a Fixed Alkali, the Liver of Sulphur formed in the operation will dissolve the martial part; so that after the fusion you will find little or no Regulus.

All Iron ores in general are refractory, and less fusible than any other; for which reason a much greater proportion of flux, and a much more violent degree of fire, is required to smelt them. One principal cause why these ores are so refractory is the property which Iron itself has of being extremely difficult to fuse, and of resisting the action of the fire so much the more as it is purer, and further removed from its mineral state. Among all the metallic substances it is the only one that is less fusible when combined with that portion of phlogiston which gives it the metalline form, than when it is deprived thereof, and in the form of a calx.

In smelting-houses Iron ore is fused amidst charcoal, the phlogiston of which combines with the martial earth, and gives it the metalline form. The Iron thus melted runs down to the bottom of the furnace, from whence it is let out into large moulds, in which it takes the shape of oblong blocks, called Pigs of Iron. This Iron is still very impure, and quite unmalleable. Its want of ductility after the first melting arises partly from hence, that, notwithstanding the previous roasting which the ore underwent, there still remains, after this first fusion, a considerable quantity of Sulphur or Arsenic combined with the metal.

A certain quantity of quick-lime, or of stones that will burn to lime, is frequently mixed with Iron ore on putting it into the smelting furnace. The lime being an absorbent earth, very apt to unite with Sulphur and Arsenic, is of use to separate those minerals from the Iron.

It is also of use to mix some such matters with the ore, when the stones or earths which naturally accompany it are very fusible; for, as the Iron is of difficult fusion, it may happen that the earthy matters mixed with the Iron shall melt as easily as the metal, or perhaps more easily. In such a case there is no separation of the earthy from the metalline part, both of which melt and precipitate together promiscuously; now quick-lime, being extremely refractory, serves on this occasion to check the melting of those matters which are too fusible.

Yet quick-lime, notwithstanding its refractory quality, may sometimes be of use as a flux for Iron. This is the case when the ore happens to be combined with substances which, being united with lime, render it fusible: such are all arsenical matters, and even some earthy matters, which being combined with quick-lime make a fusible compound.

When the ore of an Iron mine is found difficult to reduce, it is usually neglected even though it be rich: because Iron being very common, people chuse to work those mines only whose ores are smelted with the most ease, and require the least consumption of wood.

Yet refractory ores are not to be altogether rejected, when another Iron ore of a different quality is found near them. For it often happens, that two several Iron ores, which being worked separately are very difficult to manage, and yield at last but bad metal, become very tractable, and yield excellent Iron, when smelted together: and accordingly such mixtures are often made at Iron-works.

The Iron obtained from ores by the first fusion may be divided into two sorts. The one, when cold, resists the hammer, doth not easily break, and is in some measure extensible on the anvil; but, if struck with a hammer when red-hot, flies into many pieces: this sort of Iron hath always a mixture of Sulphur in it. The other sort, on the contrary, is brittle when cold, but somewhat ductile when red-hot. This Iron is not sulphurated, is naturally of a good quality, and its brittleness arises from its metalline parts not being sufficiently compacted together.

Iron abounds so much, and is so universally diffused through the earth, that it is difficult to find a body in which there is none at all: and this hath led several Chymists, even men of great fame, into the error of thinking that they had transmuted into Iron several sorts of earths in which they suspected no Iron, by combining them with an inflammable matter; whereas, in fact, all they did was to give the metalline form to a true martial earth which happened to be mixed with other earths.

PROCESS II.

To render Pig-iron and brittle Iron malleable.

Into an earthen vessel widening upwards put some charcoal-dust, and thereon lay the Pig-iron which you propose to render ductile; cover it all over with a quantity of charcoal; excite the fire violently with a pair, or more, of perpetual bellows till the Iron melt. If it do not readily flow and form a great deal of slag on its surface, add some flux, such as a very fusible sand.

When the matter is in fusion keep stirring it from time to time, that all the parts thereof may be equally acted on by the air and the fire. On the surface of the melted Iron scoriæ will be formed, which must be taken off as they appear. At the same time you will see a great many sparkles darted up from the surface of the metal, which will form a sort of fiery shower. By degrees, as the Iron grows purer, the number of these sparkles diminishes, though they never vanish entirely. When but few sparkles appear, remove the coals which cover the Iron, and let the slag run out of the vessel; whereupon the metal will grow solid in a moment. Take it out while it is still red-hot, and give it a few strokes with a hammer, to try if it be ductile. If it be not yet malleable, repeat the operation a second time, in the same manner as before. Lastly, when it is thus sufficiently purified by the fire, work it for a long time on the anvil, extending it different ways, and making it red-hot as often as there is occasion. Iron thus brought to the necessary degree of ductility, so as to yield to the hammer, and suffer itself to be extended every way, either hot or cold, without breaking to bits, or even cracking in the least, is very good and very pure. If it cannot be brought to this degree by the method here prescribed, it is a proof that the ore from which this Iron was extracted ought to be mixed with other ores; but it frequently requires a great number of trials to obtain an exact knowledge of the quality and proportion of those other ores with which it is to be mixed.

OBSERVATIONS.

The brittleness and shortness of Pig-iron arises from the heterogeneous parts which it contains, and which could not be separated from it by the first fusion. These extraneous matters are usually Sulphur, Arsenic, and unmetallic earth, and also a ferruginous earth; but such as could not be combined with the phlogiston as it ought to be, in order to have the properties of a metal, and must therefore be considered as heterogeneous, with respect to the other well-conditioned martial particles.

The Pig-iron, by undergoing repeated fusions, is freed from those heterogeneous matters; those which are volatile, such as Sulphur and Arsenic, being dissipated, and the unmetallic matters being scorified. As to the ferruginous earth, which did not at first acquire the metalline form, it becomes true Iron at last; because, among the coals with which it is encompassed, it meets with a sufficient quantity of phlogiston to reduce it to metal. Charcoal is also necessary on this occasion, that it may continually furnish phlogiston to the Iron, which would otherways be converted into a calx.

Hammering the red-hot Iron, after each fusion, serves to force out from amongst the martial parts such earthy matters as may happen to remain there, and so bring into closer contact the metalline parts which were separated before by the interposition of those heterogeneous matters.

PROCESS III.

To convert Iron into Steel.

Take small bars of the best Iron; that is, of such as is malleable both hot and cold; set them on their ends in a cylindrical earthen vessel, whose depth is equal to the length of the bars, and in such a manner that they may be an inch distant from each other, and from the sides of the crucible. Fill the vessel with a cement compounded of two parts of charcoal, one part of bones burnt in a close vessel till they become very black, and one half part of the ashes of green wood; having first pulverized and thoroughly mixed the whole together. Take care to lift up the Iron bars a little, to the end that the cement may cover the bottom of the vessel, and so that there be about the depth of half an inch thereof under every bar: cover the crucible and lute on the cover.

Set the crucible thus prepared in a furnace, so contrived that the crucible may be surrounded with coals from top to bottom: for eight or ten hours keep up such a degree of fire that the vessel may be moderately red; after this take it out of the furnace; plunge your little Iron bars into cold water, and you will find them converted into Steel.

OBSERVATIONS.

The principal difference between Iron and Steel consists in this, that the latter is combined with a greater quantity of phlogiston than the former.

It appears by this experiment, that, to make Iron unite with an inflammable matter, it is not necessary it should be in fusion; it is sufficient that it be so red-hot as to be opened and softened by the fire.

Every kind of charcoal is fit to be an ingredient in the composition of the cement employed to make Steel, provided it contain no Vitriolic Acid. However, it hath been observed, that animal coals produce a speedier effect than others: for which reason it is proper to mix something of that kind with charcoal-dust, as above directed.

The following signs shew that the operation hath succeeded, and that the Iron is changed into good Steel.

This metal being quenched in cold water, as proposed above, acquires such an extraordinary degree of hardness, that it will by no means yield to any impression of the file or hammer, and will sooner break in pieces than stretch upon the anvil. And here it is proper to observe, that the hardness of Steel varies with the manner in which it is quenched. The general rule is, that the hotter the Steel is when quenched, and the colder the water is in which you quench it, the harder it becomes. It may be deprived of the temper thus acquired, by making it red-hot, and letting it cool slowly; for it is thereby softened, rendered malleable, and the file will bite upon it. For this reason the artisans who work in Steel begin with untempering it, that they may with more ease shape it into the tool they intend to make. They afterwards new-temper the tool when finished, and by this second temper the Steel recovers the same degree of hardness it had acquired by the first temper.

The colour of Steel is not so white as that of Iron, but darker, and the grains, facets, or fibres, which appear on breaking it, are finer than those observed in Iron.

If the bars of Iron thus cemented in order to convert them into Steel be too thick, or not kept long enough in cementation, they will not be turned into Steel throughout their whole thickness: their surfaces only will be Steel to a certain depth, and the center will be mere Iron; because the phlogiston will not have thoroughly penetrated them. On breaking a bar of this sort, the difference in colour and grain between the Steel and the Iron is very visible.

It is easy to deprive Steel of the super-abundant quantity of phlogiston which constitutes it Steel, and thereby reduce it to Iron. For this purpose it need only be kept red-hot some time, observing that no matter approach it all the while that is capable of refunding to it the phlogiston which the fire carries off. The same end is still sooner obtained by cementing it with meagre hungry matters, capable of absorbing the phlogiston; such as bones calcined to whiteness, and cretaceous earths.

Steel may also be made by fusion; or Pig-iron may be converted into Steel. For this purpose the same method must be employed as was above directed for reducing Pig-iron into malleable Iron; with this difference, that, as Steel requires more phlogiston than is necessary to Iron, all the means must be made use of that are capable of introducing into the Iron a great deal of phlogiston; such as melting but a small quantity of Iron at a time, and keeping it constantly encompassed with abundance of charcoal; reiterating the fusions; taking care that the blast of the bellows directed along the surface of the metal do not remove the coals that cover it, &c. And here it must be observed, that there are some sorts of Pig-iron which it is very difficult to convert into Steel by this method, and that there are others which succeed very readily, and with scarce any trouble at all. The ores which yield the last-mentioned sort of Pig-iron are called Steel Ores. Steel made by this means must be tempered in the same manner as that made by cementation.

M. Réaumur hath obliged the public with a treatise on the means of converting Iron into Steel, in which he hath exhausted the subject. Such as desire the amplest and most useful instructions on that part of metallurgy, would do well to consult his Work.

PROCESS IV.

The Calcination of Iron. Sundry Saffrons of Mars.

Take filings of Iron, in what quantity you please; put them into a broad unglazed earthen vessel; set it under the muffle of a cupelling furnace; make it red-hot; stir the filings frequently; and keep up the same degree of fire till the Iron be wholly turned into a red powder.

OBSERVATIONS.

Iron easily loses its phlogiston by the action of fire. The calx that remains after its calcination is exceeding red; which makes this be thought the natural colour of the earth of that metal. It hath accordingly been observed, that all the earths and stones which either are naturally red, or acquire that colour by calcination, are ferruginous.

The yellowish red colour which every calx of Iron hath, in whatever manner it be prepared, hath procured the name of Crocus or Saffron to every preparation of this kind. That made in the manner above directed is called in Medicine Crocus Martis astringens.

The rust produced on the surface of Iron is a sort of calx of Iron made by way of dissolution. The moisture of the air acts upon the metal, dissolves it, and robs it of some of its phlogiston. This rust is called in Medicine Crocus Martis Aperiens; because it is thought that the saline parts, by means whereof the humidity dissolves the Iron, remain united with the metal after its dissolution, and give it an aperitive virtue. The Apothecaries prepare this sort of Saffron of Mars by exposing Iron filings to the dew, till they be turned entirely to rust: which is then called Saffron of Mars by dew.

Another Saffron of Mars is also prepared in a much shorter manner, by mixing filings of Iron with pulverized Sulphur, and moistening the mixture, which after some time ferments and grows hot. It is then set on the fire; the Sulphur burns away, and the mass is kept stirring till it become a red matter. This Saffron is nothing but Iron dissolved by the Acid of Sulphur, which is known to be of the same nature with that of Vitriol; and consequently this Saffron of Mars is no way differing from Vitriol calcined to redness.

PROCESS V.

Iron dissolved by the mineral Acids.

Put any mineral Acid whatever into a matrass with some water; set the matrass on a sand-bath gently heated; drop into the vessel some filings of Iron: the phenomena which usually accompany metalline dissolutions will immediately appear. Add more filings, till you observe the Acid hath lost all sensible action upon them: then remove your matrass from the sand-bath; you will find in it a solution of Iron.

OBSERVATIONS.

Iron is very easily dissolved by all the Acids. If you make use of the Vitriolic Acid, care must be taken to weaken it with water, in case it be concentrated; because the dissolution will succeed the better. The vapours that rise on this occasion are inflammable; and if a lighted paper be held to the mouth of the matrass, especially after keeping it stopt for some time and shaking the whole gently, the sulphureous vapours take fire with such rapidity as to produce a considerable explosion; which is sometimes strong enough to burst the vessel into a thousand pieces. This solution hath a green colour, and is in fact a fluid Green Vitriol, which wants nothing but rest to make it shoot into crystals.

If you make use of the Nitrous Acid, you must cease adding more filings when the liquor, after standing still some moments, becomes turbid; for, when this Acid is impregnated with Iron to a certain degree, it lets fall some of that which it had dissolved, and becomes capable of taking up fresh filings. Thus, by constantly adding new supplies of Iron, this Acid may be made to dissolve a much greater quantity thereof than is necessary to saturate it entirely. This solution is of a russet colour, and doth not crystallize.

If the weather be not extremely cold, and the Acids have a proper degree of strength, the sand-bath is unnecessary, as the dissolution will succeed very well without it.

Iron dissolved by Acids may be separated therefrom, like all other metallic substances in the same circumstances, either by the action of fire, which carries off the Acid and leaves the Martial Earth, or by the interposition of substances which have a greater affinity than metallic substances have with Acids; that is, by Absorbent Earths and Alkaline Salts. By whatever means you separate Iron from an Acid solvent, it constantly appears, after the separation, in the form of a yellowish red powder; because it is then deprived of most of the phlogiston to which it owed its metalline form; whence it is reasonable to think, that this is the proper colour of Martial earth.

All these precipitates of Iron are true Saffrons of Mars, which, as well as those prepared by calcination, are so much the further removed from the nature of a metal, the more they are deprived of their phlogiston. Thence it comes that they are more or less soluble by Acids, and more or less attracted by the magnet: as no ferruginous earth, perfectly deprived of all inflammable matter, is at all attracted by the magnet, or soluble by Acids.

CHAP. V.

Of TIN.

PROCESS I.

To extract Tin from its Ore.

Break your Tin ore into a coarse powder, and by washing carefully separate from it all the heterogeneous matters, and ores of a different kind, that may be mixed therewith. Then dry it, and roast it in a strong degree of fire, till no more Arsenical vapour rise from it. When the ore is roasted, reduce it to a fine powder, and mix it thoroughly with twice its weight of the black flux well dried, a fourth part of its weight of clean iron filings, together with as much borax and pitch; put the mixture into a crucible; over all put Sea-salt to the thickness of four fingers, and cover the crucible close.

Set the crucible thus prepared in a melting furnace: apply at first a moderate and slow degree of fire, till the flame of the pitch, which will escape through the joint of the cover, disappear entirely. Then suddenly raise your fire, and urge it with rapidity to the degree necessary for melting the whole mixture. As soon as the whole is in fusion take the crucible out of the furnace, and separate the Regulus from the scoria.

OBSERVATIONS.

All Tin ores contain a considerable quantity of Arsenic, and no Sulphur at all, or at most very little. Hence it comes that, though Tin be the lightest of all metals, its ore is nevertheless much heavier than any other; Arsenic being much heavier than Sulphur, of which the ores of every other kind always contain a pretty large proportion. This ore is moreover very hard, and is not brought to a fine powder with so much ease as the rest.

These properties of Tin ore furnish us with the means of separating it easily by lotion, not only from earthy and stony parts, but even from the other ores which may be mixed with it. And this is of the greater advantage on two accounts, viz. because Tin cannot endure, without the destruction of a great part thereof, the degree of fire necessary to scorify the refractory matters which accompany its ore; and again because this metal unites so easily with Iron and Copper, the ores of which are pretty commonly blended with Tin ore, that, after the reduction, it would be found adulterated with a mixture of these two metals, if they were not separated from it before the fusion.

But sometimes the Iron ore confounded with that of Tin is very heavy, and is not easily pulverized; whence it comes to pass that it cannot be separated therefrom by washing only. In that case the magnet must be employed to separate it, after the ore hath been roasted.

Roasting is moreover necessary for Tin ore, in order to dissipate the Arsenic which volatilizes, calcines, or destroys one part of the Tin, and reduces the rest to a short, brittle substance, like a Semi-metal. The ore is known to be sufficiently roasted when no more fumes rise from it; when it has lost the smell of garlic; and when it does not whiten a clean plate of Iron held over it.

Tin being one of those metals which are most easily calcined, it is necessary in reducing its ore to employ such matters as may furnish it with phlogiston. In order to defend it from the contact of the air, which always accelerates the calcination of metallic substances, the mixture is to be covered with Sea salt; and the addition of pitch helps to increase the quantity of phlogiston.

PROCESS II.

The Calcination of Tin.

Into an unglazed earthen dish put the quantity of Tin you intend to calcine; melt it, and keep stirring it from time to time. Its surface will be covered with a greyish white powder: continue the calcination till all your Tin be converted into such a powder, which is the Calx of Tin.

OBSERVATIONS.

Though the calcination of metalline substances is promoted by exposing them, in powder, or in filings, to the action of fire, and by ordering it so that they may not melt, because they present a much smaller surface when melted than when unmelted; yet we have not directed this precaution to be used in calcining Tin. The reason is, this metal is so fusible that it cannot endure the degree of fire requisite to destroy its phlogiston without melting, and of course, though Tin calcines easily, the operation is nevertheless tedious, because the melted metal presents but a small surface to be acted on by the fire and the air. This inconvenience may be partly remedied, and the operation greatly expedited, by dividing the quantity of Tin to be calcined into several small parcels, and exposing them to the fire in separate vessels, so that they may not re-unite when melted, and form one single mass.

Leaf Tin cast on Nitre in actual fusion causes it to deflagrate and fulminate; and from this mixture there rises a white vapour, which is converted into flowers when it meets with any obstacle to impede its flying off entirely.

Mr. Geoffroy, who went through a course of experiments on Tin, an account whereof may be seen in the Memoirs of the Academy of Sciences, found that from the colour of the calx of that metal a judgment may be formed of its degree of purity, and nearly of the quantity and quality of the metallic substances with which it is alloyed. The experiments tried on this subject by that eminent Chymist are very curious.

He performed the calcination in a crucible, which he heated to a cherry-red, and kept up the same degree of fire from the beginning to the end of the operation. The calx which formed upon his metal, in that degree of heat, appeared like small white scales, a little reddish on the under side. He pushed it to one side as it formed, to the end that it might not cover the surface of the metal, which, like all others, requires the contact of the air to turn it into a calx.

"While he was making these calcinations, he had an opportunity of observing a curious fact, of which no body before him had ever taken notice; probably because no body had ever calcined Tin by the same method. The fact is, that during the calcination of the Tin, whether you break the pellicle which forms on the surface of the metal while in red-hot fusion, or whether you let it remain without touching it, you perceive in several places a small swell of a certain matter, which bursts and makes its way through the pellicle. This matter puffs up, grows red, at the same instant takes fire, and darts out a small whitish flame, as vivid and as brilliant as that of Zinc, when urged by a fire strong enough to sublime it into flowers. The vividness of this flame may be further compared to that of several small grains of phosphorus of urine fired and gently dropped on boiling water. From this bright flame a white vapour exhales; after which the swelled mass partly crumbles down, and turns to a light white powder, sometimes spotted with red, according to the force of the fire. After this momentary ignition, there arise stronger, more numerous, or more frequent heavings of matter, out of which issues a good deal of white fume, that may be intercepted by a cover of tin-plate or copper fitted to the crucible, and appears to be the flowers of Tin, which in some measure corrode these metals. Hence Mr. Geoffroy conjectures, with a great deal of probability, that their sublimation is promoted by a portion of Arsenic. When the crust formed by this calx comes to be too thick, or in too great a quantity, to be pushed on one side, so as to leave part of the metal uncovered, Mr. Geoffroy puts out the fire, because no more calx would be formed: the communication of the external air with the Tin in fusion being absolutely necessary thereto, as hath been already said. In this operation it is to be observed that, if the fire be too slow, neither the inflammation of the sulphureous particles, nor the white fumes that rise, will be so distinctly perceived, as when the fire is of the degree requisite to keep the crucible just of a cherry-red heat.

"Mr. Geoffroy having taken off this first calx began the calcination anew. In this second heat the buddings or heavings were more considerable, and shot up in the form of cauli-flowers; but were still composed of little scales. The thoroughly calcined portion of this vegetation was likewise white and red; and the inferior surfaces of some little bits thereof were wholly red. When these calcinations are continued, sulphureous vapours rise seemingly of another kind than those which appeared in the beginning; for all the calx made by the first heat was perfectly white: whereas in the second it begins to be spotted here and there with a tinge of black. Mr. Geoffroy was obliged to go through a course of twelve several calcinations before he could convert two ounces of Tin into a calx. He had the opportunity, during these several calcinations, to observe that after the fourth, and sometimes after the third, the red spots of the calx decrease, and the black increase; that the germinations cease; that the crust of the calx remains flat; that in the twelfth fire the Tin yields no more of this scaly crust; that towards the end the undulations of the fused metal appear no longer; and that the small remainder of calx is mixed with several very minute grains of metal, which seem much harder than Tin. Mr. Geoffroy could not collect a sufficient quantity thereof to cupel them, and satisfy himself whether or no they were Silver."

Though Tin, and all the imperfect metals in general, seem converted to a calx, and lose the metalline form, by one single calcination, and that a slight one; yet they are not wholly deprived of their phlogiston: for if the calx of Tin, for instance, prepared according to the process above delivered, be cast upon Nitre in fusion, it will make that salt deflagrate very perceptibly; a convincing proof that it still contains much inflammable matter. If therefore a calx be required absolutely free from phlogiston, this first calx must be recalcined by a more violent fire, and the calcination continued till all the phlogiston be dissipated.

"Mr. Geoffroy, being desirous of having his calx of Tin very pure and perfectly calcined, exposed once more to the action of fire the twelve portions of calx obtained by his former calcinations. But, as it would have been too tedious to re-calcine them all separately, he made four parcels of the whole, each consisting of three taken according to the order in which they were first calcined; and gave to each a fire sufficiently strong, and long enough continued, to calcine them as thoroughly as was possible. After this second calcination he found them all of a most beautiful white, except the first parcel: as that consisted of the portions obtained by the three first heats, in all of which there were scales tinged with red, it still retained a stain of carnation, though hardly perceptible. Agreeably to the general rule, the two ounces of Tin gained in weight by being thus calcined; and the increase was two drams and fifty seven grains.

"Mr. Geoffroy observes, that no Tin, but what is absolutely pure, will yield a perfectly white calx. He calcined in this manner several other parcels of Tin that were impure and variously alloyed; each of which produced a calx differently coloured, according to the nature and quantity of its alloy: whence he justly concludes, that calcination is a very good method of trying the fineness of Tin, or its degree of purity." The particulars of Mr. Geoffroy's experiments on this subject, which are very curious, may be seen in the Memoirs of the Academy for 1738.

It is proper to take notice that a man should be very cautious how he exposes himself to the vapours of Tin, because they are dangerous; this metal being very justly suspected by Chymists of containing something Arsenical.

PROCESS III.

The dissolution of Tin by Acids, The Smoking Liquor of Libavius.

Put into a glass vessel what quantity you please of fine Tin cut into little bits. Pour on it thrice as much aqua regis, compounded of two parts aqua fortis weakened with an equal quantity of very pure water, and one part Spirit of Salt. An ebullition will arise, and the Tin will be very rapidly dissolved; especially if the quantities of metal and of aqua regis be considerable.

OBSERVATIONS.

Tin is soluble by all the Acids; but aqua regis dissolves it best of any. Yet in this dissolution it comes to pass that part of the dissolved Tin precipitates of its own accord to the bottom of the vessel, in the form of a white powder. This solution of Tin is very fit for preparing the purple-coloured precipitate of Gold. For this purpose the solution of Tin must be let fall, drop by drop, into a solution of Gold. Spirit of Nitre dissolves Tin nearly as aqua regis does; but it occasions a greater quantity of calx.

If two or three parts of Oil of Vitriol be poured on one part of Tin, and if the vessel in which the mixture is made be exposed to such a degree of heat as to evaporate all the moisture, there will remain a tenacious matter sticking to the sides of the vessel. If water be poured on this matter, and it be then exposed a second time to the fire, it will dissolve entirely, excepting a small portion of a glutinous substance, which also may be dissolved in fresh Oil of Vitriol.

The Acid of Sea-salt may be combined with Tin by the following process. Mix perfectly, by trituration in a marble mortar, an amalgam of two ounces of fine Tin, and two ounces and a half of Quick-silver, with as much Corrosive Sublimate. As soon as the mixture is completed, put it into a glass retort, and distil with the same precautions as we directed to be used in preparing concentrated and smoking Acids. There will first come over into the receiver some drops of a limpid liquor, which will be soon followed by an elastic spirit that will issue out with impetuosity. At last some flowers, and a saline tenacious matter, will rise into the neck of the retort. Then stop your distillation, and pour into a glass bottle the liquor you will find in the receiver. This liquor continually exhales a considerable quantity of dense, white fumes, as long as it is allowed to have a free communication with the air.

The product of this distillation is a combination of the Acid of Sea-salt with Tin. As the affinity of Tin with this Acid is greater than that of Mercury, the Acid contained in the Corrosive Sublimate quits the Mercury, wherewith it was united, to join the Tin; which it volatilizes so as to make it rise with itself in a limpid form. We make use of the amalgam of Tin with Quick-silver, because we are thereby enabled to mix the Corrosive Sublimate perfectly therewith, as the success of the operation requires it should be.

In this experiment the Tin is volatilized, and the Acid of Sea-salt, which is exceedingly concentrated, flies off incessantly in the form of white vapours. This compound is known in Chymistry by the name of Smoking Liquor of Libavius; a name derived from its quality, and from its Inventor. Tin dissolved by Acids is easily separated from them by Alkalis. It always precipitates in the form of a white calx.

CHAP. VI.

Of LEAD.

PROCESS I.

To extract Lead from its Ore.

Having roasted your Lead ore reduce it to a fine powder; mix it with twice its weight of the black flux, and one fourth of its weight of clean iron filings and borax; put the whole into a crucible capable of containing at least thrice as much; over all put Sea-salt four fingers thick; cover the crucible; lute the juncture; dry the whole with a gentle heat, and set it in a melting furnace.

Make the crucible moderately red: you will hear the Sea-salt decrepitate, and after the decrepitation a small hissing in the crucible. Keep up the same degree of fire till that be over.

Then throw in as many coals as are necessary to complete the operation entirely, and raise the fire suddenly, so as to bring the whole mixture into perfect fusion. Keep up this degree of fire for a quarter of an hour, which is time sufficient for the precipitation of the Regulus.

When the operation is finished, which may be known by the quietness of the matter in the crucible, and by a bright vivid flame that will rise from it, take the crucible out of the furnace, and separate the Regulus from the scoria.

OBSERVATIONS.

All Lead ore contains a good deal of Sulphur, which must be first separated from it by roasting: and as this kind of ore is apt to fly when first exposed to the fire, it is proper to keep it covered till it be thoroughly heated. Another precaution to be used, in roasting this ore, is not to give it too great a heat, but to keep the vessel which contains it just moderately red; because it easily turns clammy, which occasions it to stick to the vessel.

The Iron that is added, and mixed with the flux, absorbs the Sulphur which may happen to remain, even after roasting: it helps also to separate from the Lead some portions of semi-metal, especially of Antimony, which are frequently mixed with this ore.

There is no fear least the Iron mix with the Lead in fusion, and adulterate it: for these two metals are incapable of contracting any union together, when each has its metalline form.

Nor is there any reason to apprehend lest the Iron should, by its refractory quality, obstruct the fusion of the mixture; for though this metal be not fusible when alone, yet, by the union it contracts with the matters it is designed to absorb, it becomes so to such a degree as in some measure to perform, on this occasion, the office of a flux.

The government of the fire is a point of great consequence in this operation. It is necessary to apply but a moderate degree of heat at first: for, when the metallic earth of the Lead, combining with the phlogiston, acquires the metalline form, it swells up in such an extraordinary manner, that there is great danger least the matter should overflow, and run all out of the containing vessel. With a view therefore to avoid this inconvenience, we direct a very large crucible to be used. This heaving of the Lead, at the instant of its reduction, is attended with a noise like the whistling of wind.

Notwithstanding all the precautions that can be used to prevent the reduction from taking place too hastily, and so occasioning the effusion of the matter, it often happens that, on raising the fire in order to bring the mixture into fusion, the hissing suddenly begins again, and is very loud. In that case all the apertures of the furnace must immediately be shut close, in order to choak and suffocate the fire: for, if this be neglected, the matter in the crucible will swell up, make its way through the luting of the juncture, nay, push up the cover, and run over. This accident is to be apprehended during the first five or six minutes after you raise the fire in order to melt the mixture. This effusion of the matter is accompanied with a dull flame, a thick, grey and yellow smoke, and a noise like that of some boiling liquor. When you observe these several phenomena you may be sure the matter is run out of the crucible, either in the manner above described, or by making its way through some cracks in the vessel, and consequently that the operation is spoiled.

Moreover, this event infallibly follows whenever a bit of coal happens to fall into the crucible; and this is one reason why it is necessary to cover it.

You may be certain that the operation hath succeeded if the scoria be smooth when cold, and have not in part escaped through the lute; if the Lead be not dispersed in globules through the whole mass of the matter contained in the crucible, but is, on the contrary, collected at the bottom, in the form of a solid Regulus, not very shining, but of a blueish cast, and ductile. Moreover, the scoria ought, in the present case, to be hard and black, and should not appear full of holes like a sieve, except only in that part which was contiguous to the Salt.

Here it is proper to observe, that the Sea-salt doth not mix with the scoria, but floats upon it. After the operation it is black; which colour it gets, no doubt, from the charred parts of the flux. The absence of these signs shews the operation to have miscarried.

When the ore to be smelted is pyritose and refractory, it may be roasted at first with a much stronger degree of fire than is used for ores that are fusible; because the martial earth, and the unmetallic earth, which are always mixed in pyritose matters, hinder it from growing readily soft in the fire. Besides, such an ore requires a greater quantity of the black flux and of borax to be mixed with it, and a higher degree of fire to fuse it.

It is generally needless to mix iron filings with this sort of ore; because the martial earth, with which pyritose matters are always accompanied, is reduced during the operation by the help of the black flux, which for that purpose is mixed with it in a large proportion, and furnishes a quantity of iron sufficient to absorb the heterogeneous minerals mixed with the Lead.

Yet, if it should be observed that the pyrites which accompany the Lead ore are arsenical, then, as such pyrites contain but a small quantity of ferruginous earth, iron filings must be added; which are, on this occasion, so much the more necessary for absorbing the Arsenic, as this mineral remains in part confounded with the ore, is reduced to a Regulus during the operation, unites with the Lead, and destroys a great deal of it by procuring its vitrification.

The Lead obtained from such pyritose ores is commonly not very pure; it is blackish and scarce ductile; qualities communicated to it by a small mixture of Copper in the pyrites, which always contain more or less thereof. We shall presently shew the method of separating Lead from Copper.

Lead ore may also be reduced by melting it amidst coals. For that purpose first kindle a fire in the furnace in which you intend to melt your ore; then put a layer of your ore immediately upon the lighted coals, and cover it with another layer of coals.

Though the melting furnace used for this operation be capable of giving a considerable heat, yet it is necessary further to increase the force of the fire by the means of a good pair of perpetual bellows, which will produce an effect like that of a forge. The ore melts, the earth of the Lead unites with the phlogiston of the coals, and so is reduced to metal, which runs through the coals, and falls into an earthen vessel placed at the bottom of the furnace to receive it. Care must be taken to keep this vessel well filled with charcoal-dust, to the end that the Lead may be in no danger of calcination while it continues there; the charcoal-dust constantly furnishing it with phlogiston to preserve its metalline form.

The earthy and stony matters that accompany the ore are scorified by this fusion, just as they are by the other which is performed in a close vessel. With regard to the Sulphur and Arsenic, they are supposed to have been first accurately separated from the ore by roasting. This is the method commonly employed for smelting Lead ore at the works.

PROCESS II.

To separate Lead from Copper.

With luting earth and charcoal-dust make a flat vessel, widening upwards, and large enough to contain your metalline mass. Set it shelving downwards from the back towards the fore-part; and in the fore-part, at the bottom, make a little gutter communicating with another vessel of the same nature, placed near the former and a little lower. Let the mouth of the gutter within side the upper vessel be narrowed, by means of a small iron plate fixed across it, while the loam is yet soft; so as to leave a very small aperture, in the lower part of this canal, sufficient to discharge the Lead as it melts. Dry the whole by placing lighted coals around it.

When this apparatus is dry, put your mixed mass of Copper and Lead into the upper vessel: both in that, and in the other vessel, light a very gentle fire of wood or charcoal, so as not to exceed the degree of heat necessary to melt Lead. In such a degree of heat the Lead contained in the mixed mass will melt, and you will see it run out of the upper vessel into the lower; at the bottom of which it will unite into a Regulus. When in this degree of heat no more Lead flows, increase the fire a little, so as to make the vessel moderately red.

When no more will run, collect the Lead contained in the lower vessel. Melt it over again in an iron ladle, with a degree of fire sufficient to make the ladle red; throw into it a little tallow or pitch, and while it burns keep stirring the metal, in order to reduce any part of it that may be calcined. Remove the pellicle or thin crust which will form on the surface; squeeze out all the Lead it contains, and then put it to the mass of Copper left in the upper vessel. Check the fire, and in the same manner take off a second skin that will form on the surface of the Lead. Lastly, when the metal is ready to fix, take off the skin that will then appear on it. The Lead remaining after this will be very pure, and free from all alloy of Copper.

With regard to the Copper itself, you will find it in the upper vessel covered with a thin coat of Lead: and if the Lead mixed with it was in the proportion of a fourth or a fifth part only, and the fire applied was gentle and slow, it will retain nearly the same form after the operation that the mixed mass had before.

OBSERVATIONS.

Lead frequently remains mixed with Copper after the reduction of its ore, especially if the ore was pyritose. Though Copper be a much more beautiful and more ductile metal than Lead, yet the latter by being alloyed with the former is rendered eager and brittle. This bad quality is easily discovered by the eye on breaking it: for the surface of the broken part appears all granulated; whereas when it is pure it is more evenly, and resembles a congeries of solid angles. If the Lead be alloyed with a considerable quantity of Copper, its colour hath a yellowish cast.

Considering the bad qualities which Copper communicates to Lead, it is necessary to separate these two metals from each other. The method above laid down is the simplest and the best. It is founded on two properties belonging to Lead: the first is that of being much more fusible than Copper; so that it will melt and run in a degree of heat that is not capable of making the Copper even red-hot, which yet is very far from being able to melt it: the second is, that Lead, though it hath an affinity with Copper, and unites very perfectly therewith, yet is not able to dissolve it without a greater heat than the degree barely necessary to fuse Lead. Hence it comes that Lead may be melted in a Copper vessel, provided no greater degree of heat be applied than that purpose requires. But when the Lead becomes so hot as to be red, fume, and boil, it instantly begins to dissolve the Copper. For this reason, it is essential to the success of our operation that a moderate degree of heat only be applied, and no greater than is requisite to keep the Lead in fusion.

Charcoal-dust is made an ingredient in the composition of the vessels used on this occasion, in order to prevent the calcination of the Lead.

The iron plate, with which the entrance of the gutter within the upper vessel is narrowed, serves to prevent the larger pieces of Copper, which the Lead may carry along with it, from passing through: it stops them, and allows the Lead to run off alone.

But as these parcels of Copper may entirely choak the passage, care must be taken, when any happen to be stopt, to remove them from the entrance of the gutter, and push them back into the middle of the vessel. It is also necessary to observe whether or no the Lead fixes any where in the passage; and, if it does, the heat of that part must be increased, in order to melt it and make it run off.

Notwithstanding all the precautions that can be taken, to hinder the melted Lead from carrying off any Copper with it, it is impossible to prevent this inconvenience entirely; and therefore the Lead is melted over again, in order to separate the small portion of Copper with which it is still adulterated.

As Copper is much lighter than Lead, if these two metals happen to be so blended together that the Copper, without being in fusion and dissolved by the Lead, is only interposed between the parts of the melted Lead, so as to swim therein, it is then precisely in the case of a solid body plunged into a fluid heavier than itself, and must rise to the surface, like wood thrown into water. It is proper to burn some inflammable matter on this melted Lead, in order to reduce such parts thereof as are constantly calcining on its surface while it is in fusion; for without this precaution they would be taken off together with the Copper.

The Copper remaining after this separation is, as we took notice before, still mixed with a little Lead. If you desire to separate it entirely therefrom, you must put it into a cupel, and expose it under the muffle to such a degree of fire as may convert all the Lead into litharge. This cannot be so done but that some of the Copper also will be scorified by the heat of the fire, and by the action of the Lead: but as there is a very great difference between the facility and readiness with which these two metals calcine, the portion of Copper that is calcined, while the whole Lead is turning into litharge, is scarce worth considering.

The Lead, though carefully separated from the Copper by the process here delivered, is not yet absolutely pure: sometimes it is alloyed with Gold, and almost always contains some Silver. If you would free the Lead as much as possible from any mixture of these two metals, you must convert it into glass, separate the remaining bead, and afterwards reduce this glass of Lead. But, as these two perfect metals are of no prejudice to the Lead, it is not usual to separate them from it, unless they be in a sufficient proportion to defray the charge, and produce some profit besides.

When we examine by the cupel the just proportion of Gold and Silver that an ore or a mixed metalline mass will yield, we make a previous assay of the Lead to be employed in the operation, and afterwards, in our estimate, deduct a proper allowance for the quantity of fine metal due to the Lead made use of.

PROCESS III.

The Calcination of Lead.

Take what quantity of Lead you please; melt it in one or more unglazed earthen pans: a dark grey powder will be found on its surface. Keep stirring the metal incessantly till it be wholly converted into such a powder, which is the Calx of Lead.

OBSERVATIONS.

As Lead is a very fusible metal, and in that respect greatly resembles Tin, most of the observations we made on the calcination of Tin may be applied here.

In the calcination of all metals, and particularly in this of Lead, there appears a singular phenomenon which is not easily accounted for. It is this: though these matters lose a great deal of their substance, either by the dissipation of their phlogiston, or because some of the metal, perhaps, exhales in vapours, yet when the calcination is over their calces are found to be increased in weight, and this increase is very considerable. An hundred pounds of Lead, for example, converted into Minium, which is nothing but a calx of Lead brought to a red colour by continuing the calcination, are found to gain ten pounds weight; so that for an hundred pounds of Lead we have one hundred and ten pounds of Minium: a prodigious and almost incredible augmentation, if it be considered that, far from adding any thing to the Lead, we have on the contrary dissipated part of it.

To account for this phenomenon Natural Philosophers and Chymists have invented several ingenious hypotheses, but none of them entirely satisfactory. As we have no established theory to proceed upon, we shall not undertake to explain this extraordinary fact.

PROCESS IV.

To prepare Glass of Lead.

Take two parts of Litharge, and one part of pure crystalline Sand; mingle them together as exactly as possible, adding a little Nitre and Sea-salt: put this mixture into a crucible of the most solid and most compact earth. Shut the crucible with a cover that may perfectly close it.

Set the crucible thus prepared in a melting furnace; fill the furnace with coals; light the fire gradually, so that the whole may be slowly heated: then raise the fire so as to make the crucible very red, and bring the matter it contains into fusion; keep it thus melted for a quarter of an hour.

Then take the crucible out of the furnace, and break it: in the bottom thereof you will most commonly find a small button of Lead, and over it a transparent Glass, of a yellow colour nearly resembling that of amber. Separate this Glass from the little button of metal, and from the saline matters which you will find above it.

OBSERVATIONS.

Pure Lead, being exposed to a strong fire without any additament, turns to Litharge; which is a scaly sort of substance, more or less yellowish, shining, and soft to the touch. This is the first advance to the Vitrification of Lead. The large refineries of Gold and Silver by the means of Lead furnish a great quantity of this material. It is sometimes whitish, and is then called Litharge of Silver; sometimes yellow, and then bears the name of Litharge of Gold. The difference of its colour depends on the degree of fire it hath undergone, and on the metalline substances vitrified with it.

Litharge alone is very fusible, and being exposed to the fire is easily converted into glass: but this Glass of Lead, made without additament, is so active, so penetrating, and so apt to swell, that it can scarcely be made use of when pure. We are obliged in some sort to clog it, by uniting it with some vitrifiable matter that is not so subtile, such as sand; and it is for this reason, not to render the mixture more fusible, that we have directed the addition of one third part of Sand to two thirds of Litharge.

The Nitre and Sea-salt, prescribed as ingredients in the mixture, are designed to procure an equal fusion of the whole. For, as the sand is lighter and less fusible than the Litharge, it will partly rise towards the upper part of the crucible when that matter first begins to flow; in consequence whereof the contents of the upper part will be much more difficult to melt, and form a Glass much more compact than that below: but the Nitre and Sea-salt possessing the upper part of the crucible, because they are still lighter than the Sand, and being in their own nature very efficacious fluxes, on account of their great fusibility, they quickly bring about the fusion of those particles of sand, which, having escaped the action of the Litharge, may have risen unvitrified to its surface.

The most difficult thing to procure, and yet the most necessary to the success of this operation, is a crucible of earth so firm and compact as not to be penetrated by the Glass of Lead, which corrodes and makes its way through every thing.

The precaution of chusing a crucible, that shall contain a good deal more than the matter to be vitrified, is a necessary one, because Litharge and Glass of Lead are very apt to swell.

The rule to keep the crucible close shut is also indispensably necessary, to prevent any bit of charcoal, or other inflammable matter, from falling into it: for when this happens it occasions a reduction of the Lead, which is always attended with a sort of effervescence, and such a considerable heaving, that commonly most of the mixture runs over the crucible. For the same reason it is very proper, before you expose the mixture to the fire, to examine whether or no it contains any matter capable of furnishing a phlogiston during the operation; and if it does, to remove that matter with great care.

The little button of Lead, found at the bottom of the crucible after the operation, comes from a small portion of Lead that is commonly left in Litharge, unless you prepare it carefully yourself, and do not take it from the fire till you are sure of having destroyed all the Lead. Besides, this small portion of Lead can be of no prejudice to the operation, because it cannot communicate its phlogiston to the rest of the matter.

The revivifying of Litharge, of the Calx, and of the Glass of Lead, may be obtained by the same processes as the reduction of its ore.

PROCESS V.

Lead dissolved by the Nitrous Acid.

Put into a matrass some aqua fortis precipitated like that used to dissolve Silver; weaken it by mixing therewith an equal quantity of common water; set the matrass in a hot sand-bath; throw into it, little by little, small bits of Lead, till you see that no more will dissolve. Aqua fortis thus lowered will dissolve about a fourth of its weight of Lead.

There is gradually formed upon the Lead, as it dissolves, first a grey powder, and afterwards a white crust, which at last hinder the solvent from acting on the remaining part of the metal; and therefore the liquor should be made to boil, and the vessel should be shaken to remove those impediments, by which means all the Lead will be dissolved.

OBSERVATIONS.

Lead very much resembles Silver, with respect to the phenomena which attend its dissolution in Acids. For example, the Nitrous Acid must be very pure and uncontaminated with the Vitriolic or Marine Acid, to qualify it for keeping the Lead in solution: for, if it be mixed with either the one or the other of these Acids, the Lead will precipitate in the form of a white powder as fast as it dissolves; which is just the case with Silver.

If the Vitriolic Acid be mixed with the Nitrous, the precipitate will be a combination of the Vitriolic Acid with Lead; that is, a Neutral Metallic Salt, or Vitriol of Lead. If the Acid of Sea-salt be mixed therewith, the precipitate will be a Plumbum corneum; that is, a Metallic Salt resembling the Luna cornea.

When all the Lead is dissolved as above described, the liquor appears milky. If it be kept warm over the fire till little crystals begin to appear on its surface, and afterwards left to stand quiet, in a certain time there will be found at the bottom a greyish powder, which being tried on Gold is Mercurial enough to whiten it. Little globules of Quick-silver are even discernible in it.

We owe this observation, together with this manner of proving the existence of Mercury in Lead, and of procuring it from thence, to M. Grosse, who hath given an account of his process in the Memoirs of the Academy of Sciences, from whence we have copied the description of the operation in hand.

The solution being quickly poured off by inclination from the grey mercurial precipitate is still milky, and deposites another white sediment. When this second precipitate falls the liquor becomes clear and limpid, and is then of a fine yellow colour, like a solution of Gold. On this gold-coloured solution, and on the two precipitates above-mentioned, M. Grosse made several observations, the chief of which we shall here insert.

The yellow liquor affects the tongue at first with a taste of sweetness; but afterwards vellicates it very smartly, and leaves on it a strong sensation of acrimony, which continues for a long time.

Alkalis precipitate the Lead suspended in this liquor, just as they do all other metals dissolved by Acids; and this precipitate of Lead is white.

Sea-salt, or Spirit of Salt, separates the Lead from its solvent, and precipitates it, as we observed before, into a Plumbum corneum: but this precipitate differs from the Luna cornea, as being very soluble in water; whereas the Luna cornea will not dissolve in it at all; or at least dissolves therein with great difficulty, and in a very small quantity. This Plumbum corneum dissolved in water is again precipitated by the Vitriolic Acid. M. Grosse observes, that this forms an exception to the eighth column of Mr. Geoffroy's Table of Affinities; in which the Acid of Sea-salt is marked as having a greater affinity than any other Acid with Metallic substances.

Our solution of Lead is also precipitated in a white powder by several Neutral Salts; such as Vitriolated Tartar, Alum, and common Vitriol. It is by the means of double affinities that these Neutral Salts effect this precipitation.

Even pure water alone is capable of precipitating the Lead of our solution, by weakening the Acid, and thereby disabling it from keeping the metal suspended.

Lastly, as all the solutions of metals in Acids are nothing but Neutral Metallic Salts in a fluid form, so if the solution of Lead be evaporated over the fire, it will shoot into very beautiful crystals, about the bigness of hemp-seed, shaped like regular pyramids having square bases. These crystals are yellowish, and have a sweet saccharine taste: but what is most singular in them is, that, as they consist of the Nitrous Acid combined with Lead, which manifestly contains a great deal of phlogiston, they constitute a Nitrous Metallic Salt, which has the property of deflagrating in a crucible, without the addition of any other inflammable matter. It is extremely hard to dissolve this Salt in water.

The grey mercurial precipitate which whitens Gold, and in which little globules of running Mercury are perceivable, is far from being pure Mercury. This metallic substance makes but a small part thereof: for it is an assemblage, 1. of little crystals of the same nature with those afforded by the evaporated solution; 2. of a portion of the white matter, or powder, which renders the solution milky; 3. of a grey powder, which M. Grosse considers as the only mercurial part; 4. and lastly, of little particles of Lead that have escaped the action of the solvent; especially if a little more Lead than the Acid is capable of dissolving were added with a view to saturate it entirely, as in the present process.

By means of motion and heat the small parcels of Mercury may be amalgamated with the Lead.

That Mercury should be found entire and in globules in the Spirit of Nitre, which very easily dissolves that metallic substance, will not be surprizing to those who reflect that, in the present case, the Acid is saturated with Lead, with which it has a greater affinity than with Mercury; as appears by M. Geoffroy's Table of Affinities, where, in the column that hath the Nitrous Acid at top, Lead is placed above Mercury. Agreeably to this, if Lead be presented to a solution of Mercury in Spirit of Nitre, the Lead will be dissolved, and as the dissolution thereof advances the Mercury will precipitate.

Hence it appears that, in order to find any Mercury in the spontaneous precipitate of Lead dissolved by the Nitrous Acid, it is necessary that the Acid be entirely saturated with Lead; or else that portion of the Acid which remains unsaturated will dissolve the Mercury.

With regard to the white powder that renders the solution milky, and afterwards precipitates, it is nothing but a portion of the Lead, which, not being intimately united with the Acid, falls in part of its own accord. It is a sort of calx of Lead, which being exposed to the fire becomes partly glass, and partly Lead, because it still retains some of its phlogiston.

CHAP. VII.

Of MERCURY.

PROCESS I.

To extract Mercury from its Ore, or to revivify it from Cinabar.

Pulverize the Cinabar from which you would extract the Mercury; with this powder mix an equal part of clean iron filings; put the mixture into a retort of glass or iron, leaving at least one third part thereof empty. Set the retort thus prepared in a sand-bath, so that its body may be quite buried in the sand, and its neck decline considerably downwards: fit on a receiver half filled with water, and let the nose of the retort enter about half an inch into the water.

Heat the vessels so as to make the retort moderately red. The Mercury will rise in vapours, which will condense into little drops, and fall into the water in the receiver. When you see that nothing more comes over with this degree of heat, increase it, in order to raise what Mercury may still be left. When all the Mercury is thus brought over, take off the receiver, pour out the water contained in it, and collect the Mercury.

OBSERVATIONS.

Mercury is never mineralized in the bowels of the earth by any thing but Sulphur; with which it forms a compound of a brownish red colour, known by the name of Cinabar.

Sometimes it is only mixed with earthy and stony matters that contain no Sulphur; but, as this metallic substance is never destitute of its phlogiston, it then has its metalline form and properties. When it is found in this condition, nothing is more easy than to separate it from those heterogeneous matters. For that purpose no more is requisite than to distil the whole with a fire strong enough to raise the Mercury in vapours. This mineral is volatile; the earthy and stony matters are fixed; and a certain degree of heat will effect a complete separation of what is volatile from what is fixed.

This is not the case when Mercury is combined with Sulphur: for this latter mineral is volatile as well as Mercury; and the compound resulting from the union of them both is also volatile: so that if Cinabar were exposed to the fire in close vessels, as it must be to save the Mercury, it would be sublimed in substance, without being decomposed at all.

In order therefore to separate these two substances from each other, we must have recourse to the interposition of some third, which hath a greater affinity with one of them than the other hath, and no affinity with that other.

Iron hath all the conditions requisite for this purpose; seeing it hath, as may be seen in the Table, a much greater affinity with Sulphur than Mercury hath, and is incapable of contracting any union with Mercury.

Iron, however, is not the only substance that may be employed on this occasion: Fixed Alkalis, Absorbent earths, Copper, Lead, Silver, Regulus of Antimony, have all, as well as Iron, a greater affinity than Mercury with Sulphur. Nay, several of these substances, namely, the saline and earthy Alkalis, as well as Regulus of Antimony, cannot contract any union with Mercury: the rest, to wit, Copper, Lead, and Silver, are indeed capable of amalgamating with Mercury; but then the union which these metals contract with the Sulphur prevents it; and even though they should unite with this metallic substance, the degree of heat to which the whole mixture is exposed would soon carry up the Mercury, and separate it with ease from those fixed substances.

In this distillation the same cautions must be observed as in all others: that is, the vessels must be slowly heated, especially if a glass retort be used; the fire must be raised by degrees, and a much stronger one applied at last than at first. This operation particularly requires a very strong degree of fire, when there is but a small quantity of Mercury left.

After the operation there remains in the retort a compound of Iron and Sulphur, which may easily be converted into a crocus, by calcining it and burning away the Sulphur.

If a Fixed Alkali be employed, a Liver of Sulphur will be found in the retort after the distillation.

If the Cinabar from which you extract the Mercury be good, you will generally obtain seven eighths of its weight in Quick-silver.

In the present operation it is not necessary to lute on the receiver, because the water, in which the nose of the retort is plunged, is sufficient to fix the Mercurial vapours. In case the Cinabar, from which you intend to separate the Mercury, be mixed with a great quantity of heterogeneous, but fixed, matters, such as earths, stones, &c. it may be separated from them by subliming it with a proper degree of heat, because it is volatile.

The vapours of Mercury are prejudicial, and may excite a salivation, tremors, and palsies; they should therefore be always avoided by such as work on this mineral.

The oldest and richest mine of Mercury is that of Almaden in Spain. It is a singular property of that mine that, though the Mercury found in it is combined with Sulphur, and in the form of Cinabar, yet no additament is required to procure the separation of these two; the earthy and stony matter, with which the particles of the ore are incorporated, being itself an excellent absorbent of Sulphur.

In the Quick-silver works carried on at this mine they make no use of retorts. They place lumps of the ore on an iron grate, which stands immediately over the furnace. The furnaces which serve for this operation are closed at the top by a sort of dome, behind which stands the shaft of a chimney that communicates with the fire-place, and gives vent to the smoke. These furnaces have in their fore-side sixteen apertures, to each of which is luted an aludel in a horizontal position, communicating with a long row of other aludels placed likewise in an horizontal direction; which aludels so connected together form one long pipe or canal, the further end whereof opens into a chamber destined to receive and condense all the mercurial vapours. These rows of aludels are supported from end to end by a terrass, which runs from the body of the building, wherein the furnaces are erected, to that where the chambers are built that perform the office of receivers.

This is a very ingenious contrivance and saves much labour, expence, and trouble, that would be unavoidable if retorts were employed.

That part of the furnace which contains the lumps of ore, serves for the body of the retort; the row of aludels for its neck; and the little chambers in which these canals terminate are actual receivers. The terrass of communication, which reaches from the one building to the other, is formed of two inclined planes, the lower edges of which, meeting in the middle of the terrass, rise from thence insensibly; the one quite to the building where the furnaces are, and the other to that which forms the recipient chambers. By this means, when any Mercury escapes through the joints of the aludels, it naturally runs down along these inclined planes, and so is collected in the middle of the terrass, where the inferior sides of the planes meeting together form a sort of canal, out of which it is easily taken up.

The celebrated M. de Jussieu having viewed the whole himself, in a journey he made to this mine, furnished us with this description of the work.

PROCESS II.

To give Mercury, by the action of Fire, the appearance of a Metalline Calx.

Put Mercury into several little glass matrasses with long and narrow necks. Stop the matrasses with a little paper, to prevent any dirt from falling into them. Set them all in one sand-bath, so that they may be surrounded with sand as high as two thirds of their length. Apply the strongest degree of heat that Mercury can bear without subliming: continue this heat without interruption, till all the Mercury be turned to a red powder. The operation lasts about three months.

OBSERVATIONS.

Mercury treated according to the process here delivered hath all the appearance of a metalline calx, but it hath no more: for, if it be exposed to a pretty strong degree of fire, it sublimes, and is wholly reduced to running Mercury, without the addition of any other inflammable matter; which proves that during this long calcination it lost none of its phlogiston.

The volatile nature of Mercury, which permits it not to bear a heat of any strength without subliming, prevents our examining all the effects that fire is capable of producing on it. Yet there is reason to believe that, as this metallic substance resembles the perfect metals in its weight, its splendour, and a brilliancy which resists all the impressions of the air without alteration, it would like them be unchangeable by the greatest force of fire, if it were fixed enough to bear it.

In order to give Mercury the form of a metalline calx, it must necessarily be exposed for about three months together, to the utmost heat it can bear without subliming, as is above directed. Boerhaave kept it digesting in a less heat for fifteen years successively, both in open and in close vessels, without observing it to suffer the least change; except that there was formed upon its surface a small quantity of a black powder, which was reduced to running Mercury by trituration alone.

Mercury thus converted to a red powder is known in chymistry and medicine by the name of Mercury precipitated per se: a title proper enough, as it is actually reduced to the form of a precipitate, and that without any additament; but very improper on the other hand, considering, that in reality this Mercury is not a precipitate, as not having been separated from any menstruum in which it was dissolved.

PROCESS III.

To dissolve Mercury in the Vitriolic Acid. Turbith Mineral.

Put Mercury into a glass retort, and pour on it thrice its weight of good Oil of Vitriol. Set the retort in a sand-bath; fit on a recipient; warm the bath by degrees till the liquor just simmer. With this heat the Mercury will begin to dissolve. Continue the fire in this degree till all the Mercury be dissolved.

OBSERVATIONS.

The Vitriolic Acid dissolves Mercury pretty well: but for this purpose the Acid must be very hot, or even boil; and then too it is a very long time before the dissolution is completed. We have directed the operation to be performed in a retort; because this solution is usually employed to make another preparation called Turbith Mineral, which requires that as much as possible of the Acid solvent be abstracted by distillation. Having therefore dissolved your Mercury in the Vitriolic Acid, if you will now prepare the Turbith, you must, by continuing to heat the retort, drive over all the liquor into the receiver, and distil till nothing remains but a white powdery matter: then break the retort; pulverize its contents in a glass mortar, and thereon pour common water, which will immediately turn the white matter of a lemon-colour; wash this yellow matter in five or six warm waters, and it will be what is called in medicine Turbith Mineral; that is, a combination of the Vitriolic Acid with Mercury, five or six grains whereof is a violent purgative, and also an emetic; qualities which it possesses in common with the Vegetable Turbith, whose name it hath therefore taken.

There rises out of the retort, both while the Mercury is dissolving, and while the solvent is abstracting, a weak Spirit of Vitriol; because a great part of the Acid remains united with the Quick-silver, which at last appears in the form of a white powder: so that, if you do not incline to save the Acid which rises on this occasion, you may, instead of drawing off the liquor in a retort, evaporate it in a glass bason set on a sand-bath, which will be much sooner done.

It is very remarkable that, on this occasion, the Mercury may be exposed, without any danger of subliming, to a much greater heat than it is capable of bearing when not combined with the Vitriolic Acid; which shews that this Acid hath the property of fixing Mercury to a certain degree.

The white matter, that remains after the evaporation of the fluid, is one of the most violent corrosives, and would prove an actual poison if taken internally. By washing it several times in warm water it is freed from a great deal of its Acid, and so considerably sweetened. The proof is this; if the water used in washing the Turbith be evaporated, there remains after the evaporation a matter in form of a Salt, that being set in a cellar runs into a liquor called Oil of Mercury, which is a powerful corrosive. Several authors further direct Spirit of Wine to be burnt on the Turbith, to sweeten it still more.

If, instead of washing the white matter that remains after the moisture is drawn off, fresh Oil of Vitriol be poured on it, and then abstracted as before; this treatment being repeated two or three times, there will at last remain in the retort a matter having the appearance of an oil, which resists the action of the fire, and cannot be desiccated: qualities which are owing to the great quantity of Acid particles thus united with the Mercury. This Oil of Mercury is one of the most violent corrosives. The Mercury may be separated therefrom, by precipitating it with an Alkali, or a metallic substance that hath more affinity than Mercury with the Vitriolic Acid: Iron, for instance, may be employed in this precipitation. Mercury thus separated from the Vitriolic Acid need only be distilled to recover the form of Quick-silver.

PROCESS IV.

To combine Mercury with Sulphur. Æthiops Mineral.

Mix a dram of Sulphur with three drams of Quick-silver, by triturating the whole in a glass mortar with a glass pestle. By degrees, as you triturate, the Mercury will disappear, and the matter will acquire a black colour. Continue the triture till you cannot perceive the least particle of running Mercury. The black matter you will then have in the mortar is known in medicine by the name of Æthiops Mineral. An Æthiops may also be made by fire in the following manner.

In a shallow unglazed earthen pan melt one part of flowers of Sulphur: add three parts of running Mercury, making it fall into the pan in the form of small rain, by squeezing it through chamoy leather. Keep stirring the mixture with the shank of a tobacco-pipe all the while the Mercury is falling: you will see the matter grow thick and acquire a black colour. When the whole is thoroughly mixed, set fire to it with a match, and let as much of the Sulphur burn away as will flame.

OBSERVATIONS.

Mercury and Sulphur unite together with great ease; cold triture alone is sufficient to join them. By this means the Mercury is reduced into exceeding small atoms, and combines so perfectly with the Sulphur that the least vestige thereof is not to be seen.

Sulphur is not the only matter which being rubbed with Mercury will destroy its form and fluidity: all fat substances that have any degree of consistence, such as the fat of animals, balsams, and resins, are capable of producing the same effect. This metallic substance, being triturated for some time in a mortar with these matters, becomes at last invisible, and communicates to them a black colour. When thus divided by the interposition of heterogeneous particles, it is said to be Killed. But Mercury doth not contract such an intimate union with these other matters as it doth with Sulphur.

The Æthiops prepared by fusion is a more perfect and accurate combination of Mercury and Sulphur than the other: for, the quantity of Sulphur directed to be used in making it being much greater than is absolutely necessary to fix the Mercury, the redundant Sulphur is destroyed by burning, and none left but what is most intimately united with the Mercury; and hindered by the union it hath contracted with that metallic substance from being so easily consumed. The Æthiops therefore, which is prepared by fusion and burning the Sulphur, contains a much greater proportion of Mercury than that which is made by simple triture; so that in Medicine it ought to be prescribed in different cases, and in smaller doses.

If no more Sulphur than is just necessary to kill the Mercury be added to it at first, it will be difficult to obtain a perfect mixture; because that quantity is very small: it is better, therefore, to employ at once the quantity above directed.

PROCESS V.

To sublime the Combination of Mercury and Sulphur into Cinabar.

Grind to powder Æthiops mineral prepared by fire. Put it into a cucurbit; fit thereto a head; place it in a sand-bath, and begin with applying such a degree of heat as is requisite to sublime Sulphur. A black matter will rise, and adhere to the sides of the vessel. When nothing more will rise with this degree of heat, raise the fire so as to make the sand and the bottom of the cucurbit red; and then the remaining matter will sublime in the form of a brownish red mass, which is true Cinabar.

OBSERVATIONS.

Æthiops Mineral requires nothing but sublimation to become true Cinabar, like that found in Quick-silver mines: but our Æthiops contains still more Sulphur than ought to be in the composition of Cinabar; for which reason we have directed the degree of fire applied at first to be no greater than that which is capable of subliming Sulphur. As Cinabar, though consisting of Mercury and Sulphur, is yet much less volatile than either of these substances alone; which probably arises from the Vitriolic Acid contained in the Sulphur; therefore, if there be any redundant Sulphur in the Æthiops, which hath not contracted an intimate union with the Mercury, it will sublime by itself in this first degree of heat. Some mercurial particles also will rise with it, and give it a black colour.

Cinabar contains no more Sulphur than about a sixth or seventh part of its weight: so that, instead of employing the common Æthiops to make it, it would be better to prepare one on purpose that should contain much less Sulphur; because too much Sulphur prevents the success of the operation by blackening the Sublimate. Indeed in whatever manner you go about it, the Cinabar always appears black at first: but when it is well prepared, and contains no more than its due proportion of Sulphur, the blackness is only external. This black coat therefore may be taken off; and then the internal part will appear of a fine red, and, if sublimed a second time, will be very beautiful.

As artificial Cinabar hath the same properties with the native, it may be decomposed by the same means: so that, if you want to extract the Mercury out of it, recourse must be had to the process above delivered for working on Cinabar ores.

PROCESS VI.

To dissolve Mercury in the Nitrous Acid. Sundry Mercurial Precipitates.

Put into a matrass the quantity of Mercury you intend to dissolve: pour on it an equal quantity of good Spirit of Nitre, and set the matrass in a sand-bath moderately heated. The Mercury will dissolve with the phenomena that usually attend the dissolutions of metals in this Acid. When the dissolution is completed let the liquor cool. You will know that the Acid is perfectly saturated, if there remain at the bottom of the vessel, notwithstanding the heat, a little globule of Mercury that will not dissolve.

OBSERVATIONS.

Mercury dissolves in the Nitrous Acid with much more facility, and in much greater quantity, than in the Vitriolic; so that it is not necessary, on this occasion, to make the liquor boil. This solution when cold yields crystals, which are a Nitrous Mercurial Salt. If you desire to have a clear limpid solution of Mercury, you must employ an aqua fortis that is not tainted with the Vitriolic or Marine Acid: for, the affinity of these two Acids with Mercury being greater than that of the Nitrous Acid, they precipitate it in the form of a white powder, when they are mixed with the solvent.

Mercury thus precipitated in a white powder, out of a solution thereof in the Spirit of Nitre, is used in Medicine. To obtain this precipitate, which is known by the name of the White Precipitate, Sea-salt dissolved in water together with a little Sal Ammoniac is used; and the precipitate is washed several times in pure water, without which precaution it would be corrosive, on account of the great quantity of the Marine Acid which it would contain.

The preparation known by the name of Red Precipitate is also obtained from our solution of Mercury in Spirit of Nitre. It is made by abstracting all the moisture of the solution, either by distillation in a retort, or by evaporation in a glass bason set on a sand-bath. When it begins to grow dry it appears like a white ponderous mass. Then the fire is made strong enough to drive off almost all the Nitrous Acid, which, being now concentrated, rises in the form of red vapours. If these vapours be catched in a receiver, they condense into a liquor, which is a very strong and vastly smoking Spirit of Nitre.

By degrees, as the Nitrous Acid is forced up by the fire, the mercurial mass loses its white colour, and becomes first yellow, and at last very red. When it is become entirely of this last colour the operation is finished. The red mass remaining is a Mercury that contains but very little Acid, in comparison of what it did while it was white: and indeed the first white mass is such a violent corrosive, that it cannot be used in Medicine; whereas, when it is become red, it makes an excellent escharotic, which those who know how to use it properly apply with very great success, particularly to venereal ulcers.

This preparation is very improperly called a Precipitate: for the Mercury is not separated from the Spirit of Nitre by the interposition of any other substance, but only by evaporating the Acid. It is also called Arcanum Corallinum.

It must be observed that Mercury, by its union with the Nitrous Acid, acquires a certain degree of fixity: for the red precipitate is capable of sustaining, without being volatilized, a stronger degree of heat than pure Mercury can; which, as we observed before, is the property of Turbith Mineral also.

PROCESS VII.

To combine Mercury with the Acid of Sea-salt. Corrosive Sublimate.

Evaporate a solution of Mercury in the Nitrous Acid till there remain only a white powder, as mentioned in our observations on the preceding process. With this powder mix as much Green Vitriol calcined to whiteness, and as much decrepitated Sea-salt, as there was Mercury in the solution. Triturate the whole carefully in a glass mortar. Put this mixture into a matrass, so that two thirds thereof may remain empty, having first cut off the neck to half its length: or instead thereof you may use an apothecary's phial. Set your vessel in a sand-bath, and put sand round it as high as the contents can reach. Apply a moderate fire at first, and raise it by slow degrees. Vapours will begin to ascend. Continue the fire in the same degree till they cease. Then stop the mouth of the vessel with paper, and increase the fire till the bottom of the sand-bath be red-hot. With this degree of heat a Sublimate will rise, and adhere to the inside and upper part of the vessel, in the form of white, semi-transparent crystals. Keep up the fire to the same degree till nothing more will sublime. Then let the vessel cool; break it, and take out what is sublimed, which is Corrosive Sublimate.

OBSERVATIONS.

In this operation the mineral Acids act, and are acted upon, in a remarkable manner. Every one of the three is at first neutralized, or united with a different basis; the Vitriolic being combined with Iron; the Nitrous with Mercury, forming therewith a Nitrous Mercurial Salt; and the Marine with its natural Alkaline basis. The Vitriolic and Nitrous Acids, which are united with metalline substances, being both stronger than the Acid of Sea-salt, strive to expel it from its basis, in order to combine with it themselves; but the Vitriolic Acid, being the strongest of the two, would take sole possession of this basis exclusive of the Nitrous, which would continue united with the Mercury, if the Marine Acid had not a greater affinity than the Nitrous with this metallic substance. This Acid therefore being expelled from its basis by the Vitriolic Acid, and so set at liberty, must unite with the Mercury, and separate the Nitrous Acid from it; which now hath no resource but to unite with the Iron deserted by the Vitriolic Acid. But as all these changes are brought about by the means of a considerable heat, and as the Nitrous Acid hath not a very firm connection with the Iron, it is driven off by the force of the fire; and this it is which we see rise in vapours during the operation. It also carries off with it some parts of the other two Acids, but in a very small quantity. After the operation therefore there remains, 1. A combination of the Vitriolic Acid with the basis of Sea-salt; that is, a Glauber's Salt: 2. A red martial earth, being that which was the basis of the Vitriol: these two substances are blended together, and remain at the bottom of the vessel because of their fixity: 3. A combination of the Marine Acid with Mercury; both of which being volatile, they ascend together into the upper part of the vessel, and there form a Corrosive Sublimate.

If we reflect on this process with attention, and recollect distinctly the affinities of the different substances employed in it, we shall perceive that it is not necessary to make use of all those matters, and that the operation would succeed though several of them were left out.

First, the Nitrous Acid may be omitted; since, as hath been shewn, it is not an ingredient in the Sublimate, but is dissipated in vapours during the operation. From an accurate mixture therefore of Vitriol, Sea-salt, and Mercury, a Corrosive Sublimate must be obtained: for as the Acid of the Vitriol will disengage the Acid of Sea-salt, the latter will be at liberty to combine with the Mercury, and so form the compound we are in quest of.

Secondly, if we make use of Mercury dissolved by the Nitrous Acid, we may omit the Vitriol; because the Nitrous Acid having a greater affinity than the Marine Acid itself with the basis of Sea-salt, and the Acid of Sea-salt having a greater affinity than the Nitrous Acid with Mercury, these two Acids will naturally make an exchange of the bases with which they are united: the Nitrous will lay hold on the basis of Sea-salt, and form a quadrangular Nitre, while the Marine Acid will join the Mercury, and with it form a Corrosive Sublimate.

Thirdly, instead of Sea-salt its Acid only may be employed; which being mixed with the solution of Mercury in the Spirit of Nitre, will, by virtue of its greater affinity with that metallic substance, separate it from the Nitrous Acid, unite with it, and form a white mercurial precipitate, which need only be sublimed to become the combination required.

Fourthly, instead of Mercury dissolved in the Nitrous Acid, Mercury dissolved by the Vitriolic Acid, or Turbith, may be used; only mixing Sea-salt therewith: for these two saline substances will mutually decompound each other, by virtue of the affinities of their Acids, and for the same reasons that Sea-salt and the Mercurial Nitrous Salt decompound each other. The Vitriolic Acid quits the Mercury with which it is combined, to unite with the basis of the Sea-salt; and the Acid of this Salt being expelled by the Vitriolic, combines with the Mercury, and consequently forms our Corrosive Sublimate. In this case a Glauber's Salt remains after the sublimation.

These several methods of preparing Corrosive Sublimate are never used, because each of them is attended with some inconvenience; such as requiring too long triture, yielding a Sublimate less corrosive than it should be, or a smaller quantity of it. We must, however, except the last; which was invented by the late Mr. Boulduc, of the Academy of Sciences, who found none of these inconveniencies attending it.

See the Memoirs of the Academy for 1730.

Corrosive Sublimate may also be made only by mixing Mercury with Sea-salt, without any additament. This may appear surprizing when we consider that, as Acids have a greater affinity with Alkalis than with metallic substances, the Acid of Sea-salt ought not to quit its basis, which is Alkaline, to unite with Mercury.

In order to explain this phenomenon it must be remembered that Sea-salt, when exposed to the fire without additament, suffers a little of its Acid to escape. Now this portion of the Marine Acid unites with the Mercury, and forms a Corrosive Sublimate. Moreover, as there is a pretty strong affinity between the Marine Acid and Mercury, this may help to detach from the Sea-salt a greater quantity of Acid than it would otherwise part with. Nevertheless, the quantity of Sublimate obtained by this means is not considerable, nor is it very corrosive.

On this occasion we must also mention another combination of the Marine Acid with Mercury; which is made by mixing that metallic substance perfectly with Sal Ammoniac, by the means of triture. Mercury, like all other metals except Gold, possesses the property of decompounding Sal Ammoniac, separating the volatile Alkali which serves it for a basis, and combining, by the help of a very gentle heat, with its Acid, which is well known to be the same with that of Sea-salt. This decomposition of Sal Ammoniac, by the metalline substances, is a full exception to the first column of Mr. Geoffroy's Table of Affinities, and is the basis of several new Medicines invented by the late Comte de la Garaye.

See the Memoir given in by me on this subject to the Academy of Sciences in the Memoires l'Acadamie 1754.

Corrosive Sublimate is the most violent and the most active of all corrosive poisons. It is never used in Medicine, but in external applications. It is a powerful escharotic; it destroys proud flesh, and cleans old ulcers: but it must be used by those only who know how to apply it properly, and requires an able hand to manage it. It is not commonly applied by itself, but mixed in the proportion of half a dram to a pound of lime-water. This mixture is yellowish, and bears the name of Aqua Phagadenica.

Water dissolves Corrosive Sublimate, but in a small quantity. If a Fixed Alkali be mixed with this solution, the Mercury precipitates in the form of a red powder. If the precipitate be procured by a Volatile Alkali, it is white; if by Lime-water, it is yellow. This Mercurial Salt dissolves pretty easily in boiling Spirit of Wine.

PROCESS VIII.

Sweet Sublimate.

Take four parts of Corrosive Sublimate; pulverize it in a glass or marble mortar; add by little and little three parts of Mercury revivified from Cinabar; triturate the whole carefully, till the Mercury be perfectly killed, so that no globule thereof can be perceived. The matter will then be grey. Put this powder into an apothecary's phial, or into a matrass, whose neck is not above four or five inches long, leaving two thirds thereof empty. Set the vessel in a sand-bath, and put sand round it to one third of its heighth. Apply a moderate fire at first; and afterwards raise it gradually till you perceive that the mixture sublimes. Keep it up to this degree till nothing more will rise, and then break the vessel. Reject, as useless, a small quantity of earth which you will find at the bottom; separate also what adheres to the neck of the vessel, and carefully collect the matter in the middle, which will be white. Pulverize it; sublime it a second time, in the same manner as before; and in the same manner separate the earthy matter left at the bottom of the vessel, and what you find sublimed into the neck. Pulverize, and sublime a third time, the white matter you last found in the middle. The white matter of this third sublimation is the Sweet Sublimate, called also Aquila Alba.

OBSERVATIONS.

The Acid of Sea-salt in the Corrosive Sublimate is very far from being perfectly saturated with Mercury; and thence comes the corrosive quality of this saline compound. But though Mercury, as appears by this combination, is capable of imbibing a much greater quantity of Acid than is necessary to dissolve it; nay, though it naturally takes up this super-abundant quantity of Acid, yet it doth not follow from thence that this redundant Acid may not combine with Mercury to the point of perfect saturation, so as to lose its corrosive acidity.

This is the case in the operation here described. A fresh quantity of running Mercury is mixed with Corrosive Sublimate; and the fresh Mercury, combining with the super-abounding Acid, deprives the Sublimate of its acrimony, and forms a compound which comes much nearer the nature of a Neutral Metallic Salt.

Trituration alone is not sufficient to produce an union between the newly added Mercury and the Acid of the Corrosive Sublimate: because, generally speaking, the Acid of Sea-salt cannot dissolve Mercury without the help of a certain degree of heat, and unless it be reduced into vapours.

Thus, though the newly added Mercury becomes invisible by trituration, and seems actually combined with the Corrosive Sublimate, yet the union is not intimate. There is only an interposition of parts, but no true dissolution of the newly added Mercury by the super-abundant Acid of the Corrosive Sublimate. For this reason the mixture must be sublimed; and by this sublimation only is the true union effected. Nor is one single sublimation sufficient: no less than three are necessary to deprive the Sublimate of the corrosive quality which renders it poisonous. After the third sublimation, the Sublimate being put upon the tongue gives no considerable sensation of acrimony; nor doth it retain any more of its former activity than is requisite to make it a gentle purgative, when administered from six to thirty grains for a dose.

If a less quantity of Mercury than that above directed be mixed with the Corrosive Sublimate, the super-abundant Acid will not be sufficiently saturated; and the less Mercury is added, the more of its corrosive virtue will the Sublimate retain.

If, on the contrary, a greater quantity of Mercury be added, there will be more than the Acid can possibly dissolve, and the superfluous quantity will remain in its natural form of Quick-silver. It is better therefore to err in the excess than in the defect of the proportion of Mercury to be added; because the Corrosive Sublimate will take up no more than is necessary to dulcify it.

Part of the Acid of the Corrosive Sublimate is also dissipated in vapours during the operation; and it is necessary to allow room for these vapours to circulate, and a vent to give them passage, or else they will burst the vessels. These are our reasons for leaving an empty space in the subliming vessels, and for having their necks no more than five or six inches long.

The matter which sublimes into the neck of the vessel is always very acrid; for which reason it must be separated from the Sweet Sublimate. There remains also at the bottom of the matrass an earthy, reddish matter; which probably comes from the Vitriol employed in making the Corrosive Sublimate. This matter must likewise be rejected as useless after every sublimation.

PROCESS IX.

The Panacea of Mercury.

Pulverize some Sweet Sublimate, and sublime it in the same manner as you did thrice before. Repeat this nine times. After these sublimations it will make no impression on the tongue. Then pour on it aromatic Spirit of Wine, and set the whole in digestion for eight days. After that decant the Spirit of Wine, and dry what remains, which is the Panacea of Mercury.

OBSERVATIONS.

The great number of sublimations, which the Sweet Sublimate is made to undergo, sweeten it still more, and to such a degree that it leaves no sensation on the tongue, nor hath any purgative virtue.

The Spirit of Wine in which it is digested after all the sublimations, is designed to blunt still more the sharpness of any acid particles that may not have been sufficiently dulcified by the preceding sublimations.

As Mercury is the specific remedy for venereal disorders, sundry preparations thereof have been attempted with a view to produce different effects. Sweet Sublimate is purgative; and for that reason is not quite proper for procuring a salivation, because it carries off the humours by stool. The Panacea of Mercury, which, on the contrary, is not purgative, may raise a salivation when taken inwardly.

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