PART I. Of MINERALS. (continued 2)

"If the air rushes out with too much rapidity, and with a hissing noise, the door of the ash-hole must be entirely shut, in order to slacken the fire. If it do not strike pretty smartly against the hand, that door must be opened wider, and large coals thrown into the fire-place to quicken the fire immediately.

"The operation usually lasts four and twenty hours; and the following signs shew that it will succeed, provided the retort resist the fire.

"You must begin the operation with putting some unlighted charcoal in the ash-hole, and a little lighted charcoal at the door thereof, in order to warm the retort very slowly. When the whole is kindled, push it into the ash-hole, and close the door thereof with a tile. This moderate heat brings over the phlegm of the mixture. The same degree of fire must be kept up four hours, after which some coals may be laid on the grate of the fire-place, which the fire underneath will kindle by degrees. With this second heat brought nearer the retort, the ballon grows warm, and is filled with white vapours, which have the smell of fetid oil. In four hours after, this vessel will grow cool and clear; and then you must open the door of the ash-hole one inch, throw fresh coals into the fire-place every three minutes, and every time shut the door of it, lest the cold air from without should strike against the bottom of the retort and crack it.

"When the fire has been kept up to this degree for about two hours, the inside of the ballon begins to be netted over with a volatile salt of a singular nature, which cannot be driven up but by a very violent fire, and which smells pretty strong of peach-kernels. Care must be taken that this concrete salt do not stop the little hole in the ballon: for in that case it would burst, the retort being then red-hot, and the air exceedingly rarefied. The water in the ballon, being heated by the vicinity of the furnace, exhales vapours which dissolve this sprigged salt, and the ballon clears up in half an hour after it has ceased rising.

"In about three hours from the first appearance of this salt, the ballon is again filled with new vapours, which smell like Sal Ammoniac thrown upon burning coals. They condense on the sides of the receiver into a salt which is not branched like the former, but appears in long perpendicular streaks, which the vapours of the water do not dissolve. These white vapours are the fore-runners of the Phosphorus, and a little before they cease to rise they lose their first smell of Sal Ammoniac, and acquire the odour of garlic.

"As they ascend with great rapidity, the little hole must be frequently opened, to observe whether the hissing be not too strong: for, in that case, it would be necessary to shut the door of the ash-hole quite close. These white vapours continue two hours. When you find they cease rising, make a small passage through the dome, by opening some of its registers, that the flame may just begin to draw. Keep up the fire in this mean state till the first volatile Phosphorus begin to appear.

"This appears in about three hours after the white vapours first begin to rise. In order to discover it, pull out the little birchen peg once every minute, and rub it against some hot part of the furnace, where it will leave a trail of light, if there be any Phosphorus upon it.

"Soon after you observe this sign, there will issue out through the little hole of the ballon a stream of blueish light, which continues of a greater or shorter extent to the end of the operation. This stream or spout of light does not burn. If you hold your finger against it for twenty or thirty seconds, the light will adhere to it; and if you rub that finger over your hand, the light will besmear it, and render it luminous.

"But from time to time this streamer darts out to the length of seven or eight inches, snapping and emitting sparks of fire; and then it burns all combustible bodies that come in its way. When you observe this, you must manage the fire very warily, and shut the door of the ash-hole quite close, yet without ceasing to throw coals into the fire-place every two minutes.

"The Volatile Phosphorus continues two hours; after which the little spout of light contracts to the length of a line or two: and now is the time for pushing your fire to the utmost: immediately set the door of the ash-hole wide open, throw billets of wood into it, unstop all the registers of the reverberatory, supply the fire-place with large coals every minute: in short, for six or seven hours all the inside of the furnace must be kept of a white heat, so that the retort shall not be distinguishable.

"In this fierce extremity of heat the true Phosphorus distils like an oil, or like melted wax: one part thereof floats on the water in the recipient, the other falls to the bottom. At last, the operation is known to be quite over when the upper part of the ballon, in which the volatile Phosphorus appears condensed in a blackish film, begins to grow red: for this shews that the Phosphorus is burnt where the red spot appears. You must now stop all the registers, and shut all the doors of the furnace, in order to smother the fire; and then close up the little hole in the ballon with fat lute or bees-wax. In this condition the whole must be left for two days; because, the vessels must not be separated till they are perfectly cold, lest the Phosphorus should take fire.

"As soon as the fire is out, the ballon, which is then in the dark, presents a most agreeable object: all the empty part thereof above the water seems filled with a beautiful blue light: which continues for seven or eight hours, or as long as the ballon keeps warm, never disappearing till it is cooled.

"When the furnace is quite cold take out the vessels, and separate them from each other as neatly as possible. With a linen cloth wipe away all the black stuff you find in the mouth of the ballon; for if that filth should mix with the Phosphorus, it would hinder it from being transparent when moulded. This must be done with great expedition: after which pour into the ballon two or three quarts of cold water, to accelerate the precipitation of the Phosphorus that swims at top. Then agitate the water in the ballon, to rinse out all the Phosphorus that may stick to the sides: pour out all the water thus shaken and turbid, into a very clean earthen pan, and let it stand till it grows clear. Then decant this first useless water, and on the blackish sediment, left at the bottom of the pan, pour some boiling water to melt the Phosphorus; which thereupon unites with the fuliginous matter, or volatile Phosphorus, that precipitated with it, both together forming a mass of the colour of slate. When this water, in which you have melted the Phosphorus, is cool enough, take out the Phosphorus, throw it into cold water, and therein break it into little bits in order to mould it.

"Then take a matras, having a long neck somewhat wider next the body than at its mouth: cut off half the body, so as to make a funnel of the neck-part, the smaller end of which must be stopped with a cork. The first mould being thus prepared, plunge it endwise, with its mouth uppermost, in a vessel full of boiling water, and fill it with that water. Into this funnel throw the little bits of your slate-like mass, which will melt again in this hot water, and fall so melted to the bottom of the tube. Stir this melted matter with an iron wire, to promote the separation of the Phosphorus from the fuliginous matter with which it is fouled, and which, being less ponderous than the Phosphorus, will gradually rise above it towards the upper part of the cylinder.

"Keep the water in the vessel as hot as at first, till, on taking out the tube, you see the Phosphorus clean and transparent. Let the clear tube cool a little, and then set it in cold water, where the Phosphorus will congeal as it cools. When it is perfectly congealed, pull out the cork, and with a small rod, near as big as the tube, push the cylinder of Phosphorus towards the mouth of the funnel, where the feculency lies. Cut off the black part of the cylinder, and keep it apart: for when you have got a quantity thereof, you may melt it over again in the same manner, and separate the clean Phosphorus which it still contains. As to the rest of the cylinder which is clean and transparent, if you intend to mould it into smaller cylinders, you may cut it in slices, and melt it again by the help of boiling water in glass tubes of smaller dimensions."

OBSERVATIONS.

This process for making Phosphorus is copied from the Memoirs of the Academy of Sciences for the Year 1737; where it is described by M. Hellot, with so much accuracy, clearness, and precision, that I thought I could not do better than transcribe it, without departing from the author's own expressions, for the sake of such as may not have those Memoirs. We shall take occasion, in these observations, to point out some essential circumstances which I have omitted in the description of the Process, that I might not break the connection between the phenomena that happen in the course of this experiment.

It is proper to observe, in the first place, that one of the most usual causes of miscarriage in this operation is a defect of the requisite qualities in the retort employed. It is absolutely necessary to have that vessel made of the best earth, and so well made that it shall be capable of resisting the utmost violence of fire, continued for a very long time; as appears by the description of the process. The retorts commonly sold by potters, and other earthen-ware men, are not fit for this operation; and M. Hellot was obliged to send to Hesse-Cassel for such as he wanted.

We shall, in the second place, observe with M. Hellot, that, "before you set your retort in the furnace, it is proper to make an essay of your matter, to see if there be reason to hope for success. For this purpose put about an ounce thereof into a small crucible, and heat it till the vessel be red. The mixture, after having smoked, ought to chop or crack without puffing up, or even rising in the least. From these cracks will issue undulating flames, white and blueish, darting upwards with rapidity. This is the first volatile Phosphorus, which occasions all the danger of the operation. When these first flashes are over, increase the heat of your matter by laying a large live coal upon the crucible. You will then see the second Phosphorus, like a luminous, steady vapour, of a colour inclining to violet, covering the whole surface of the matter: it continues for a very long time, and diffuses a smell of garlic, which is the distinguishing odour of the Phosphorus you are seeking.

"When this luminous vapour is entirely gone, pour the red hot matter out of the crucible upon an iron plate. If you do not find one drop of salt in fusion, but that, on the contrary, the whole falls readily into powder, it is a proof that your matter was sufficiently lixiviated, and that it contains no more fixed Salt, or Sea-salt, if you will, than is requisite. If you find on the plate a drop of salt coagulated, it shews that there is too much left in, and that there is danger of your miscarrying in the operation; because the redundant salt would corrode, and eat through the retort. In this case your matter must be washed again, and then sufficiently dried."

Our third observation shall be concerning the furnace proper to be employed in this operation. This furnace must be so constructed, that, within a narrow compass it may give a heat at least equal to that of a glass-house furnace, or rather greater, especially during the last seven or eight hours of the operation. M. Hellot in his Memoir gives an exact description of such a furnace.

"As certain accidents may happen in the course of the operation, some precautions are to be taken against them. For instance, if the ballon should break while the Phosphorus is distilling, and any of it should fall on combustible bodies, it would set them on fire, and probably burn the laboratory, because it is not to be extinguished without the greatest difficulty. The furnace must therefore be erected under some vault, or upon a bed of brick-work raised under some chimney that draws well: nor must any furniture or utensil of wood be left near it. If a little flaming Phosphorus should fall on a man's legs or hands, in less than three minutes it would burn its way to the very bone. In such a case nothing but urine will stop its progress.

"If the retort crack while the Phosphorus is distilling, there is an unsuccessful end of your operation. It is easy to perceive this by the stink of garlic which you will smell about the furnace; and moreover, the flame that issues through the apertures of the reverberatory will be of a beautiful violet colour. The Acid of Sea-salt always gives this colour to the flame of such matters as are burnt along with it. But if the retort break before the Phosphorus hath made its appearance, its contents may be saved by throwing a number of cold bricks into the fire-place, and upon them a little water to quench the fire at once." All these useful observations we owe also to M. Hellot.

The Phosphorus here described was first discovered by a citizen of Hamburgh, named Brandt, who worked upon urine in search of the Philosopher's stone. Afterwards two other skilful Chymists, who knew nothing more of the process, than that Phosphorus was obtained from urine, or, in general, from the human body, likewise endeavoured to discover it; and each of them separately did actually make the discovery. These two Chymists were Kunckel and Boyle.

The former perfected the discovery, and found out a method of making it in considerable quantities at a time; which occasioned it to be called Kunckel's Phosphorus. The other, who was an English gentleman, had not time to bring his discovery to perfection, and contented himself with lodging a voucher of his having discovered it in the hands of the Secretary of the Royal Society of London, who gave him a certificate thereof.

"Though Brandt," says M. Hellot, "who had before this sold his secret to a Chymist named Krafft, sold it afterwards to several other persons, and even at a very low rate; and though Mr. Boyle published the process for making it; yet it is extremely probable that both of them kept in their own hands the master-key; I mean, the particular management necessary to make the operation succeed: for, till Kunckel found it out, no other Chymist ever made any considerable quantity thereof, except Mr. Godfrey Hankwitz, an English Chymist, to whom Mr. Boyle revealed the whole mystery.

"Nevertheless," continues he, "we are very far from alledging that all those who have described this operation meaned to impose upon the world: but we conceive that most of them having observed luminous vapours in the ballon, and some sparks about the juncture of the vessels, were contented with those appearances. And thus it came to pass, that, after Kunckel and Boyle died, Mr. Godfrey Hankwitz was the only Chymist that could supply Europe therewith; on which account it is likewise very well known by the name of English Phosphorus."

Almost all the Chymists consider Phosphorus as a substance consisting of the Acid of Sea-salt combined with the Phlogiston, in the same manner as Sulphur consists of the Vitriolic Acid combined with the Phlogiston. This opinion is founded on the following principles.

First, Urine abounds with Sea-salt, and contains also a great deal of Phlogiston; now these are the ingredients of which they conjecture Phosphorus to be composed.

Secondly, Phosphorus has many of the properties of Sulphur; such as being soluble in oils; melting with a gentle heat; being very combustible; burning without any soot; giving a vivid and blueish flame; and lastly, leaving an acid liquor when burnt: sensible proofs that it differs from Sulphur in nothing but the nature of its Acid.

Thirdly, this Acid of Phosphorus, being mixed with a solution of silver in Spirit of Nitre, precipitates the silver, and this precipitate is a true Luna cornea, which appears to be more volatile even than the common sort; as M. Hellot tells us, who made the experiment. This fact proves incontestably that the Acid of Phosphorus is of the same nature with that of Sea-salt: for all Chymists know that the property of precipitating silver in a Luna cornea belongs to the Marine Acid only.

Fourthly, M. Stahl observes, that, if Sea-salt be cast on live coals, they instantly burn with great activity; then they emit a very vivid flame, and are much sooner consumed than if none of this salt had touched them; that Sea-salt in substance, which will bear the violence of fire a considerable time when fused in a crucible, without sustaining any sensible diminution, yet evaporates very quickly, and is reduced to white flowers, by the immediate contact of burning coals; and, lastly, that the flame which rises on this occasion is of a blue colour inclining to violet, especially if it be not thrown directly on the coals themselves, but kept in fusion amidst burning coals, in a crucible so placed that the vapour of the Salt may join with the enflamed Phlogiston as it rises from the coals.

These experiments of M. Stahl's prove, that the Phlogiston acts upon the acid of Sea-salt, even while it is combined with its alkaline basis. The flame that appears on this occasion may be considered as an imperfect Phosphorus: and indeed its colour is exactly like that of Phosphorus.

All the facts above related evince, that the Acid of Phosphorus is akin to that of Sea-salt; or rather that it is the very same. But there are other facts which prove that this Acid undergoes some change at least, some peculiar preparation, before it enters into the composition of a true Phosphorus, and that, when extricated therefrom by burning, it is not a pure Acid of Sea-salt, but is still adulterated with a mixture of some other substance, which makes it considerably different from that Acid. For these observations we are obliged to M. Marggraff, of the Academy of Sciences at Berlin, a celebrated Chymist. I shall presently give an account of his principal experiments as succinctly as possible.

M. Marggraff hath also published a process for making Phosphorus, and assures us, that by means thereof we may obtain in less time, with less heat, less trouble, and less expence, a greater quantity of Phosphorus than by any other method. His operation is this:

He takes two pounds of Sal Ammoniac in powder, which he mixes accurately with four pounds of Minium. This mixture he puts into a glass retort, and with a graduated fire draws off a very sharp, volatile, urinous spirit.

We observed in our theoretical Elements, that some metallic substances have the property of decomposing Sal Ammoniac, and separating its volatile Alkali; concerning which phenomenon we there gave our opinion. Minium, which is a calx of lead, is one of those metallic substances. In this experiment it decomposes the Sal Ammoniac, and separates its volatile Alkali; what remains in the retort is a combination of the Minium with the Acid of the Sal Ammoniac, which is well known to be the same with the Marine Acid; and consequently the residue of this operation is a sort of Plumbum corneum.

The quantity thereof is four pounds eight ounces. Of this he mixes three pounds with nine or ten pounds of urine, that has stood putrefying for two months, evaporated to the consistence of honey. These he mixes by little and little in an iron pan over the fire, stirring the mixture from time to time. Then he adds half a pound of charcoal-dust, and evaporates the matter, kept continually stirring, till the whole be brought to a black powder. He next distils the mixture in a glass retort with degrees of fire, which he raises towards the end so as to make the retort red-hot, in order to expel all the urinous spirit, superfluous oil, and ammoniacal salt. The distillation being finished, there remains nothing in the retort but a very friable caput mortuum.

This remainder he pulverises again, and throws a pinch thereof on live coals, thereby to discover whether or no the matter be rightly prepared, and in order for yielding Phosphorus. If it be so, it presently emits an arsenical odour, and a blue undulating flame, which passes over the surface of the coals like a wave.

Being thus assured of the success of his operation, he puts one half of his matter in three equal parts, into three small earthen German retorts, capable of holding about eighteen ounces of water a-piece. These three retorts, none of which is above three quarters full, he places together in one reverberatory furnace, built much like those we have described, except that it is so constructed as to hold the three retorts disposed in one line. To each retort he lutes a recipient something more than half full of water, ordering the whole in such a manner, that the noses of his retorts almost touch the surface of the water.

He begins the distillation with warming the retorts slowly, for about an hour, by a gentle heat. When that time is elapsed he raises the fire gradually, so that in half an hour more the coals begin to touch the bottoms of the retorts. He continues throwing coals into the furnace by little and little, till they rise half way the heighth of the retorts; and in this he employs another half hour. Lastly, in the next half hour he raises the coals above the bowls of the retorts.

Then the Phosphorus begins to ascend in clouds: on this he instantly increases the heat of the fire as much as possible, filling the furnace quite up with coals, and making the retorts very red. This degree of fire causes the Phosphorus to distil in drops, which fall to the bottom of the water. He keeps up this intense heat for an hour and half, at the end of which the operation is finished; so that it lasts but four hours and an half in all: nay, he further assures us, that an artist well versed in managing the fire, may perform it in four hours only. In the same manner he distils the second moiety of his mixture in three other such retorts.

The advantage he finds in making use of several small retorts, instead of a single large one, is, that the heat penetrates them with more ease, and the operation is performed with less fire, and in less time. He purifies and moulds his Phosphorus much in the same manner as M. Hellot does. From the quantity of ingredients above-mentioned, he obtains two ounces and a half of fine crystalline moulded Phosphorus.

M. Marggraff considering, as a consequence of the experiments above related, that a highly concentrated Acid of Sea-salt contributes greatly towards the formation of Phosphorus, proceeded to try several other experiments, in which he employed that Acid in a state of combination with other bases. He mixed, for instance, an ounce of Luna cornea with an ounce and half of putrefied and inspissated urine, and from the mixture obtained a very beautiful Phosphorus.

In short, the several experiments mentioned having thoroughly persuaded him that the Acid of Sea-salt, provided it were highly concentrated, would combine with the Phlogiston as readily as the Vitriolic Acid does, he resolved to try whether he could not make Phosphorus with matters containing that Acid and the Phlogiston, without making use of any urine.

With this view he made a great number of different trials, wherein he employed Sea-salt in substance, Sal Ammoniac, Plumbum corneum, Luna cornea, fixed Sal Ammoniac, otherwise called Oil of Lime. These several substances, all of which contain the Acid of Sea-salt, he mixed with sundry matters abounding in Phlogiston, different vegetable coals, and even animal matters, such as the oil of hartshorn, human blood, &c. varying the proportions of these substances many different ways, without ever being able to produce a single atom of Phosphorus: which gave this able Chymist just cause to suspect, that the Marine Acid, while pure and crude, is not capable of combining with the Phlogiston in the manner requisite to form a Phosphorus; that for this purpose it is necessary the Acid would have contracted a previous union with some other matter; and that the Acid found in urine hath probably undergone the necessary change. M. Marggraff is of opinion that the matter, which by its union renders the Marine Acid capable of entering into the composition of Phosphorus, is a sort of exceedingly subtle vitrifiable earth. The experiments he made upon the Acid of Phosphorus, will shew that his notion is not altogether groundless. M. Marggraff having let some urine, evaporated to the consistence of honey, stand quiet in a cool place, obtained from it, by crystallization, a Salt of a singular nature. By distilling this urine afterwards, he satisfied himself that it yielded him much less Phosphorus than urine from which no Salt had been extracted; and as it cannot be entirely deprived of this Salt, he thinks that the small quantity of Phosphorus, which this urine yielded him, came from the Salt that was still left in it.

Further, he distilled this salt separately with lamp-black, and obtained from it a considerable quantity of very fine Phosphorus. He even mixed Luna cornea with this Salt, in order to see whether it would not increase the quantity of his Phosphorus; but without success: whence he concluded, that in this Saline matter resides the true Acid that is fit to enter into the composition of Phosphorus. This opinion is confirmed by several experiments on the Acid of Phosphorus, which he found to have some properties resembling those of this Salt.

The Acid of Phosphorus seems to be more fixed than any other: and therefore if you would separate it, by burning, from the Phlogiston with which it is united, there is no occasion for such an apparatus of vessels as is employed for obtaining the Spirit of Sulphur. For this Acid will remain at the bottom of the vessel in which you burn your Phosphorus: indeed, if it be urged by the force of fire, its most subtile part evaporates, and the remainder appears in the form of a vitrified matter.

This Acid effervesces with fixed and volatile Alkalis, and therewith forms Neutral Salts; but very different from Sea-salt, and from Sal Ammoniac. That which has a fixed Alkali for its basis does not crackle when thrown on burning coals; but swells and vitrifies like Borax. That which has a volatile Alkali for its basis shoots into long pointed crystals; and, being urged by fire in a retort, lets go its volatile alkali, a vitrified matter remaining behind. This Salt is like that above-mentioned, as obtained from urine and yielding Phosphorus.

It appears from the experiments adduced, that the Acid of Phosphorus tends always to vitrification; which proves that it is not pure, and gave M. Marggraff cause to think that it is altered by the admixture of a very subtile vitrifiable earth.

M. Marggraff also obtained Phosphorus from several vegetable substances which we use every day for food. This gives him occasion to conjecture, that the Salt requisite to the formation of Phosphorus exists in vegetables, and passes from thence into the animals that feed upon them.

Lastly, he concludes his dissertation by informing us of a very important truth, viz. That the Acid obtained from Phosphorus, by burning it, will serve to form Phosphorus anew; for which purpose it need only be combined with some charred coal, such as lamp-black, and distilled.

From what hath been said on this subject it is plain, that the Chymists have a great many curious and interesting inquiries to make concerning Phosphorus, and particularly concerning its Acid.

I shall conclude this article with an account of certain properties of Phosphorus which I have not yet mentioned.

Phosphorus dissolves by lying exposed to the air. What water cannot effect, says M. Hellot, or at least requires eight or ten years to bring about, the moisture of the air accomplishes in ten or twelve days; whether it be that the Phosphorus takes fire in the air, and the inflammable part evaporating, almost entirely, leaves the Acid of the Phosphorus naked, which, like all other Acids, when exceedingly concentrated, is very greedy of moisture; or else that the moisture of the air, being water divided into infinitely fine particles, is so subtile as to find its way through the pores of the Phosphorus, into which the grosser particles of common water can by no means insinuate themselves.

Phosphorus heated by the vicinity of fire, or by being any way rubbed, soon takes fire and burns fiercely. It is soluble in all Oils and in Ether, giving to those liquors the property of appearing luminous when the bottle containing the solution is opened. Being boiled in water, it likewise communicates thereto this luminous quality. M. Morin, Professor at Chartres, is the author of this observation.

The late Mr. Grosse, a celebrated Chymist of the Academy of Sciences, observed, that Phosphorus being dissolved in essential oils crystallizes therein. These crystals take fire in the air, either when thrown into a dry vessel, or wrapt up in a piece of paper. If they be dipped in Spirit of Wine, and taken out immediately, they do not afterwards take fire in the air: they smoke a little, and for a very short time, but hardly waste at all. Though some of them were left in a spoon for a fortnight, they did not seem to have lost any thing of their bulk: but when the spoon was warmed a little they took fire, just like common Phosphorus that had never been dissolved and crystallized in an essential Oil.

M. Marggraff, having put a dram of Phosphorus, with an ounce of highly concentrated Spirit of Nitre, into a glass retort, observed, that, without the help of fire, the Acid dissolved the Phosphorus; that part of the Acid came over into the recipient which was luted to the retort; that, at the same time, the Phosphorus took fire, burnt furiously, and burst the vessels with explosion. Nothing of this kind happens when any of the other Acids, though concentrated, are applied to Phosphorus.

PROCESS III.

To decompose Sea-salt by means of the Vitriolic Acid. Glauber's Salt. The Purification and Concentration of Spirit of Salt.

Put the Sea-salt from which you mean to extract the Acid into an unglazed earthen pipkin, and set it amidst live coals. The Salt will decrepitate, grow dry, and fall into a powder. Put this decrepitated Salt into a tubulated glass retort, leaving two thirds thereof empty. Set the retort in a reverberating furnace; apply a receiver like that used in distilling the Smoking Spirit of Nitre, and lute it on in the same manner, or rather more exactly if possible. Then through the hole, in the upper convexity of the retort, pour a quantity of highly concentrated Oil of Vitriol, equal in weight to about a third part of your Salt, and immediately shut the hole very close with a glass stopple, first ground therein with emery so as to fit it exactly.

As soon as the Oil of Vitriol touches the Salt, the retort and receiver will be filled with abundance of white vapours; and soon after, without lighting any fire in the furnace, drops of a yellow liquor will distil from the nose of the retort. Let the distillation proceed in this manner without fire, as long as you perceive any drops come: afterwards kindle a very small fire under the retort, and continue distilling and raising the fire by very slow degrees, and with great caution, to the end of the distillation; which will be finished before you have occasion to make the retort red-hot. Unlute the vessels, and without delay pour the liquor, which is a very smoking Spirit of Salt, out of the receiver into a crystal bottle, like that directed for the smoking Spirit of Nitre.

OBSERVATIONS.

Sea-Salt, as hath been already said, is a Neutral Salt composed of an Acid, which differs from those of Vitriol and Nitre, combined with a fixed Alkali that has some peculiar properties; but does not vary from the others in its affinities. This Salt therefore, as well as Nitre, must be decomposed by the Vitriolic Acid; which accordingly is the case in the process here described. The Vitriolic Acid unites with the Alkaline basis of the Sea-salt, and separates its Acid; and that with much greater facility than it expels the Nitrous Acid from its Alkaline basis, because the Acid of Sea-salt has not so great an affinity as the Nitrous Acid with Fixed Alkalis.

As a highly concentrated Oil of Vitriol is used on this occasion, and as the Sea-salt is previously dried and decrepitated, the Acid obtained from it by distillation is very free from phlegm, and always smokes, even more violently than the strongest Acid of Nitre. The vapours of this Acid are also much more elastic and more penetrating than those of the Nitrous Acid: on which account this distillation of the smoking Spirit of Salt is one of the most difficult, most laborious, and most dangerous operations in Chymistry.

This process requires a tubulated retort, that the Oil of Vitriol may be mixed with the Sea-salt after the receiver is well luted to the retort, and not before: for, as soon as these two matters come together, the Spirit of Salt rushes out with so much impetuosity, that, if the vessels were not luted at the time, the copious vapours that would issue through the neck of the ballon would so moisten it, as well as the neck of the retort, that it would be impracticable to apply the lute and secure the joint as the operation requires. Moreover, the operator would be exposed to those dangerous fumes, which, on this occasion, rush out, and enter the lungs, with such incredible activity as to threaten instant suffocation.

Having said so much of the elasticity and activity of the fumes of Spirit of Salt, it is needless to insist upon the necessity of giving vent to the vessels from time to time, by opening the little hole of the ballon: indeed the best way to prevent the loss of a great many vapours, on this occasion, is to employ adopters, and cover them with wet canvas, which will cool and condense the vapours they contain.

When the operation is finished, we find a white, saline mass at the bottom of the retort as in a mould. If this mass be dissolved in water, and the solution crystallized, it yields a considerable quantity of Sea-salt that hath not been decomposed, and a Neutral Salt consisting of the Vitriolic Acid united with the Alkaline basis of that part which hath been decomposed. This Neutral Salt, which bears the name of Glauber its inventor, differs from Vitriolated Tartar, or the Sal de duobus, which remains after distilling the Nitrous Acid, especially in that it is more fusible, more soluble in water, and hath its crystals differently figured. But as in these two Salts the Acid is the same, the differences that appear between them must be attributed to the peculiar nature of the basis of Sea-salt.

Spirit of Salt drawn by the process above described is tainted with a small mixture of the Vitriolic Acid, carried up by the force of fire before it had time to combine with the Alkali of the Sea-salt; which happens likewise to the Nitrous Acid procured in the same manner. If you desire to have it pure, and absolutely free from the Acid of Vitriol, it must be distilled a second time from Sea-salt, as the Acid of Nitre was before directed to be distilled again from fresh Nitre, in order to purify it from any Vitriolic taint.

Sea-salt, as well as Nitre, may be decomposed by any combination of the Vitriolic Acid with a metallic or earthy substance: but it is proper to observe, that if you distil Spirit of Salt by means of Green Vitriol, the operation will not succeed so well as when Spirit of Nitre is distilled in the same manner: less Spirit is obtained, and a much fiercer fire is required.

The cause of this lies in the property which the Acid of Sea-salt possesses of dissolving Iron, even when deprived of a part of its Phlogiston by having contracted an union with another Acid; so that it is no sooner dislodged from its own basis by the Vitriolic Acid, than it unites with the ferruginous basis of the Vitriol, from which it cannot be separated but by a most violent fire. This is the consequence more especially when calcined Vitriol is made use of: for moisture, as we shall presently see, greatly facilitates the separation of the Marine Acid from those substances with which it is united.

When you do not desire a highly dephlegmated and smoking Spirit of Salt, you may distil with the additament of any earth containing the Vitriolic Acid; as Clay, for instance, or Bole. To this end one part of Sea-salt, slightly dried and reduced to a fine powder, must be accurately mingled with two parts of the earth you intend to employ likewise pulverized; of this mixture make a stiff paste with a proper quantity of rain water, and having formed little balls thereof about the size of a hazel nut, let them dry in the sun; when dry, put them into a stone or coated glass retort, leaving a third part thereof empty; set this vessel in a reverberating furnace, covered with its dome; apply a receiver, which need not be luted on for some time; and heat the vessels very slowly. At first an insipid water will rise, which must be thrown away: afterwards the Spirit of Salt will appear in white clouds. Now lute your vessels, and raise the fire by degrees; which, towards the end must be pushed to the utmost extremity. The operation is known to be finished when no drops fall from the nose of the retort, the receiver cools, and the white vapours that filled it are seen no more.

The Spirit of Salt obtained by the process here delivered does not smoke, and contains much more phlegm than that which is distilled by means of the concentrated Oil of Vitriol; because the earth, though dried in the sun, still retains a great deal of moisture, which commixes with the Acid of the Sea-salt. Consequently it is much easier to collect its vapours; so that this operation is attended with much less trouble than the other. Nevertheless it is adviseable to proceed gently; to apply but little heat at first, and to unstop every now and then the small hole of the receiver: for a quantity of the vapours of Spirit of Salt, even when weakened by the admixture of water, is very apt to burst the vessels.

A much greater degree of fire is necessary to raise the Spirit of Salt by this latter process, than by that in which the pure Vitriolic Acid is employed: for, as fast as the Spirit of Salt is dislodged from its own basis, by the Vitriolic Acid contained in the earth made use of, part of it joins that earth, and cannot be separated from it without the most violent heat.

A Spirit of Salt that shall not smoke may also be obtained by means of the pure Vitriolic Acid. Spirit of Vitriol, or Oil of Vitriol, lowered with a good deal of water, will do the business.

Some Chymists direct a little water to be placed in the receiver, when Spirit of Salt is to be distilled by the intermedium of concentrated Oil of Vitriol, in order to make the acid vapours condense more readily. By this means indeed some of the inconveniencies attending the distillation of smoking Spirit of Salt may be avoided: but, on the other hand, the acid vapours being absolutely suffocated by the water as fast as they come over, the Spirit of Salt obtained by this method will be no less aqueous than that procured by the interposition of earths: so that here is an expence to no manner of purpose. Therefore, when a Spirit of Salt is desired that shall not smoke, it is best to employ an additament of earth; and that so much the rather as the Marine Acid obtained by this means is purer and freer from any Vitriolic taint, for the reasons already assigned.

Part of the Acid of Sea-salt may be separated from its Alkaline basis by the force of fire alone, without the intervention of any other body. With this view the Salt must be put into the retort without being dried. At first an insipid water rises; but it gradually becomes acid, and hath all the properties of Spirit of Salt. When the Salt in the retort is grown perfectly dry, nothing more can be forced over by any degree of heat whatever. If you would obtain more Acid from the same Salt, you must take it out of the retort, where you will find it in a lump, reduce it to powder, and expose it to the air for some time, that it may attract the moisture thereof; or else wet it at once with some rain water, and distil as before. You will again have an insipid water, and a little Spirit of Salt; which will in like manner cease to rise when the Salt in the retort becomes dry. This operation may be repeated as often as shall be thought proper: and perhaps it may be possible to decompose Sea-salt entirely by means thereof, without the interposition of any other body. The Spirit of Salt thus obtained is exceeding weak, in small quantity, and loaded with much water.

This experiment proves, that moisture greatly facilitates the separation of the Acid of Sea-salt from the matters with which it is united: and this is the reason that, in distilling Spirit of Salt with the additament of an earth, the operation requires much less fire at the beginning, while the earth and salt retain a great deal of humidity, than towards the end, when they begin to grow dry.

After the operation there remains in the retort a saline and earthy mass, which contains, 1. Some entire Sea-salt that has suffered no decomposition; 2. A Glauber's Salt which is, as we said before, a Neutral Salt consisting of the Vitriolic Acid united with the Alkaline basis of the Sea-salt, from which it hath expelled its proper Acid; 3. Part of the earth used as an intermedium, still retaining a portion of its original Vitriolic Acid, which happening not to lie near enough to any particles of Sea-salt, could not exert its power in decomposing them, and so remains united with its earthy basis; 4. Another part of the same earth, impregnated with some of the Marine Acid, which combined therewith upon being expelled from its Alkaline basis by the Vitriolic Acid, and which the force of fire was unable to separate from it when the matters were grown perfectly dry. In consequence of what remains in this caput mortuum, if the whole mass be triturated, moistened with a little water, and distilled a second time, considerably more Spirit of Salt will be obtained from it: and the same is to be said of all distillations of this sort.

Spirit of Salt obtained by the means of any other additament than concentrated Oil of Vitriol is generally very weak: but it may be dephlegmated and concentrated, if required, much in the same manner as Oil of Vitriol. For this purpose you must put it into a glass cucurbit, set it in a balneum mariæ, fit thereto a head and a receiver, and with a moderate degree of heat draw off one third or one half of the liquor. What comes over into the receiver will be the most aqueous part, which being the lightest will rise first, impregnated however with a little acid: in the cucurbit will be left a concentrated Spirit of Salt, or the most acid part, which being the heaviest will not rise with the degree of heat that is capable of carrying up the phlegm. Spirit of Salt thus concentrated, called also Oil of Salt, does not smoke: it is of a yellow colour inclining to green, and an agreeable smell, not unlike that of saffron.

PROCESS IV.

To decompose Sea-salt by means of the Nitrous Acid. Aqua regis. Quadrangular Nitre.

Take dried Sea-salt; bruise it to powder; put it into a glass retort, leaving one half of the vessel empty. Pour upon it a third of its weight of good Spirit of Nitre. Place your retort in the sand-bath of a reverberating furnace; put on the dome; lute to the retort a receiver having a small hole in it, and heat the vessels very slowly. There will come over into the receiver some vapours, and an acid liquor. Increase the fire gradually till nothing more rises. Then unlute the vessels, and pour the liquor out of the receiver into a crystal bottle, stopped like others containing Acid Spirits.

OBSERVATIONS.

The Nitrous Acid hath a greater affinity than the Marine Acid with fixed Alkalis. When therefore Spirit of Nitre and Sea-salt are mixed together, the same consequences, in some measure, will follow, as when the Vitriolic Acid is mixed with that salt; that is, the Nitrous Acid will, like the Vitriolic, decompose it, by dislodging its Acid from its Alkaline basis, and assuming its place. But as the Nitrous Acid is considerably weaker, and much lighter, than the Vitriolic Acid, a good deal of it rises along with the Acid of Sea-salt during the operation. The liquor found in the receiver is therefore a true Aqua regis.

If decrepitated Salt, and a right smoking Spirit of Nitre, be employed in this process, the Aqua regis obtained will be very strong; and, during the operation, very elastic vapours will rush out and burst the vessels, if those precautions be not taken which we pointed out as necessary in distilling the Spirit of Nitre, and the smoking Spirit of Salt.

The operation being finished, there is left in the retort a saline mass, containing Sea-salt not decomposed, and a new species of Nitre, which having for its basis the Alkali of Sea-salt, that is, as we have several times observed, an Alkali of a peculiar nature, differs from the common Nitre, 1. In the figure of its crystals; which are solids of four sides, formed like lozenges: 2. In that it crystallizes with more difficulty, retains more water in its crystals, attracts the moisture of the air, and dissolves in water with the same circumstances as Sea-salt.

CHAP. IV.

Of Borax.

PROCESS.

To decompose Borax by the means of Acids, and to separate from it the Sedative Salt by sublimation and by crystallization.

Reduce to a fine powder the Borax from which you intend to extract the Sedative Salt. Put this powder into a wide-necked glass retort. Pour upon it an eighth part of its weight of common water, to moisten the powder; and then add concentrated Oil of Vitriol to the weight of somewhat more than a fourth part of the weight of Borax. Set the retort in a reverberatory, make a moderate fire at first, and augment it gradually till the retort become red-hot.

A little phlegm will first come over, and then with the last moisture that the heat expels the Sedative Salt will rise; by which means some of it will be dissolved in this last phlegm, and pass therewith into the receiver; but most of it will adhere in the form of saline flowers to the fore-part of the neck of the retort, just where it is clear of the groove of the furnace. There they collect into a heap, which the succeeding flowers push insensibly forward till they slightly stop the passage. Those which rise after the neck is thus stopped stick to the after-part of it which is hot, vitrify in some measure, and form a circle of fused Salt. In this state the flowers of the Sedative Salt seem to issue out of the circle, as from their basis: they appear like very thin, light, shining scales, and must be brushed off with a feather.

At the bottom of the retort will be left a saline mass: dissolve this in a sufficient quantity of hot water; filter the solution in order to free it from a brown earth which it deposites; set the liquor to evaporate, and crystals of Sedative Salt will form in it.

OBSERVATIONS.

Though Borax is of great use in many chymical operations, especially in the fusion of metals, as we shall have occasion to see, yet, till of late years, Chymists were quite ignorant of its nature, as they still are of its origin; concerning which we know nothing with certainty, but that it comes rough from the East Indies, and is purified by the Dutch.

M. Homberg was one of the first that attempted to analyse this Salt. He shewed, that on mixing it with the Vitriolic Acid, and distilling the mixture, a salt sublimes in little fine needles. This product of Borax he called by the name of Sedative Salt, because he found it had the property of moderating the great tumult and heat of the blood in fevers.

After M. Homberg, other Chymists also exercised themselves on Borax. M. Lemery discovered that the Vitriolic is not the only Acid by means of which the Sedative Salt may be obtained from Borax; but that either of the other two Mineral Acids, the Nitrous or the Marine, may be used in its stead.

M. Geoffroy hath greatly facilitated the means of obtaining the Sedative Salt from Borax; having shewn that it may be extracted by crystallization as well as by sublimation; and that the Sedative Salt so obtained is in no respect inferior to that which was procured before by sublimation only. To him also we are indebted for the discovery, that in the composition of Borax there is an Alkaline Salt of the same nature as the basis of Sea-salt. This he found by observing that he got a Glauber's Salt from a solution of Borax into which he had poured some Vitriolic Acid with a view to obtain its Sedative Salt.

Lastly, M. Baron, whom we mentioned before on occasion of this Salt, hath proved, by a great number of experiments, that a Sedative Salt may be procured from Borax by the help of Vegetable Acids, which was never done by any body before him; that the Sedative Salt is not a combination of an Alkaline matter with the Acid made use of in extracting it, as some of its properties seemed to indicate; but that it exists previously and completely formed in the Borax; that the Acid employed to extract it only helps to disengage it from the Alkali with which it is united; that this Alkali is actually of the same nature as the basis of Sea-salt, because that after extracting the Sedative Salt, which by its union therewith forms the Borax, a Neutral Salt is found, of the same sort with that which would be produced by combining the basis of Sea-salt with the particular Acid made use of; that is, if with the Vitriolic Acid, a Glauber's Salt; if with the Nitrous Acid, a quadrangular Nitre; and if with the Marine Acid, a true Sea-salt; and, lastly, that the Sedative Salt may be re-united to its Alkali, and reproduce a Borax.

Nothing therefore now remains, to give us all the insight we can desire into the nature of Borax, but to know what the Sedative Salt is. M. Baron hath already given us certain negative notices concerning it, by shewing what it is not; that is, that the Acid employed in its extraction doth not enter into its composition. We have great reason to hope, that he will carry his inquiries still further, and clear up all our doubts on this subject.

The Sedative Salt may be extracted from Borax, not only by the means of pure and simple Acids, but also by the same Acids combined with a metallic basis. Thus Vitriols, for instance, may be employed for this purpose with good success. It is easy to see, that the Vitriol must be decomposed on this occasion, and that its Acid cannot unite with the Alkali in which the Sedative Salt is lodged, without quitting its metallic basis, which must of course precipitate.

The Sedative Salt actually sublimes, when a liquid containing it is distilled; but it does not therefore follow, that it is naturally volatile. It rises only by the aid of the water with which it is mixed. The proof of this assertion is, that, when all the humidity of the mixture containing this Salt is dissipated, no more Salt will rise, be the fire ever so violent; and that by adding more water to moisten the dried mass containing it, more Salt will every time be obtained, through many repeated distillations. In the same manner, if some Sedative Salt be moistened, and exposed to a proper degree of heat, a small quantity thereof will rise at first by the help of the water; but as soon as it grows dry it remains exceedingly fixed. This observation we owe to M. Rouelle.

The Sedative Salt hath the appearance and the taste of a Neutral Salt: it does not change the colour of the juice of violets; nor does it easily dissolve in water; for it requires a quart of boiling water to dissolve two ounces of it: yet, with regard to Alkalis, it has the properties of an Acid; it unites with those salts, forms therewith a saline compound which crystallizes, and even expels the Acids that happen to be combined with them; so that it decomposes the same Neutral Salts that are decomposed by the Vitriolic Acid.

The Sedative Salt, when suddenly exposed to the violent heat of a naked fire, loses near half its weight, melts, puts on and retains the appearance of glass; but its nature still remains unchanged. This glass dissolves in water, and shoots anew into crystals of Sedative Salt. This Salt communicates to the Alkaline salt with which it is united, when in the form of Borax, the property of melting with a moderate heat, and forming a kind of glass; and it is this great fusibility that recommends the frequent use of Borax as a flux for assaying ores. It is also employed sometimes as an ingredient in the composition of glass; but, in time, it always communicates thereto the fault which its own glass hath, namely that of tarnishing with the air. The Sedative Salt hath, moreover, the singular property of dissolving in Spirit of Wine, and of giving to its flame, when set on fire, a beautiful green colour. All these observations we owe to Mess. Geoffroy and Baron.

M. Geoffroy prepares the Sedative Salt by crystallization only, in the following manner. "He dissolves four ounces of refined Borax in a sufficient quantity of warm water, and then pours into the solution one ounce and two drams of highly concentrated Oil of Vitriol, which makes a crackling noise as it falls in. When this mixture has stood evaporating for some time, the Sedative Salt begins to make its appearance in little, fine, shining plates floating on the surface of the liquor. The evaporation is then to be stopped, and the plates will by little and little increase in thickness and breadth. They unite together into little tufts, forming with each other sundry different groups. If the vessel be ever so little stirred, the regularity of the crystals will be disturbed; so that it must not be touched till the crystallization appears to be finished. The crystalline clusters, being grown too bulky and too heavy, will then fall of themselves to the bottom of the vessel. This being observed, the saline liquor must be gently decanted from those little crystals, which, as they are not easily dissolved, must be washed clean, by pouring cold water slowly on the sides of the pan, three or four times successively, in order to rinse out all remains of the saline liquor, and then set first to drain, and afterwards to dry in the sun. This Salt, in the form of light flakes of snow, is now soft to the touch, cool in the mouth, slightly bitter, crackling a little between the teeth, and leaving a small impression of acidity on the tongue. It will keep long without giving or calcining, if managed according to the preceding directions; that is, if it be exactly freed from its saline liquor.

"It differs from the Sedative Salt obtained by sublimation in this respect only, that notwithstanding its seeming lightness it is a little heavier than the other. M. Geoffroy supposes the cause of this weight to be, that, as several of the thin plates adhere together in crystallizing, they retain between them some small matter of humidity; or, if you will, that, as they form larger crystals, they present less surface to the air which elevates light bodies: whereas, on the contrary, the other Sedative Salt, being driven up by the force of fire, rises into the head of the cucurbit in a more subtile form, having its particles much more expanded and divided.

"M. Geoffroy, having put his Sedative Salt made by crystallization to all the same trials with that made by sublimation, satisfied himself that there is no other difference between the two. If the Sedative Salt made by crystallizations happens to calcine in the sun; that is, if its lustre tarnishes, and its surface grows mealy, it is a sign that it still contains either a little Borax or some Glauber's Salt: for these two Salts are apt to calcine in this manner, and pure Sedative Salt should not be subject to this inconvenience. In order to purify it, and free it entirely from those Salts, it must be dissolved once more in boiling water. As soon as the water cools, the Sedative Salt reappears in light, shining, crystalline plates, swimming in the liquor. After standing four and twenty hours, the liquor must be decanted, and the salt washed with fresh water; by which means it will be very pure and beautiful."

Glauber's Salt and Borax dissolve in water with vastly more ease than the Sedative Salt, and consequently do not crystallize so readily by much: so that the small portion of those salts which may have been left on the surface of the Sedative Salt, being diffused through a large quantity of water, continues in a state of solution, while the Sedative Salt crystallizes; which being also washed afterwards with fair water, it is impossible that the smallest particle of those other Salts should remain adhering to it; and consequently this must be deemed an excellent way of purifying it.

SECTION II.

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.