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[9].
[9] 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[10].
[10] 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.
SECTION III.
_Of Operations on the_ SEMI-METALS.
CHAP. I.
_Of_ ANTIMONY.
PROCESS I.
_To Separate Antimony from its Ore by Fusion._
Having drilled some small holes, of about two lines in diameter, in
the bottom of a crucible, put into it your Antimonial Ore broken into
little bits, about the size of a hazel nut; lute on its cover; set the
crucible thus prepared in the mouth of another crucible, and close the
joints with lute.
At the distance of half a foot from this compound vessel place bricks
all round, so as to form a furnace; the sides of which must rise as
high as the brim of the uppermost crucible.
Let the bottom of this furnace be filled with ashes, up to the top of
the lower crucible, and the rest of the furnace with lighted coals.
Blow the fire, if it be necessary, with bellows, till the upper
crucible become red. Keep it up in this degree for about a quarter of
an hour. Then take your vessels out of the furnace, and you will find
the Antimony collected in the bottom of the lower crucible, having run
through the holes of the upper one.
_OBSERVATIONS._
The ore of Antimony is one of the most fusible: it always contains a
great deal of Sulphur, and cannot sustain a fire of any force without
being dissipated into vapours. It requires no additament to flux it:
for it is not necessary, on this occasion, that the earthy and stony
matters mixed therewith be brought to fusion. It is sufficient that
the Antimonial part be melted; which, as soon as it becomes fluid, is
carried by its weight to the lower part of the crucible. Thus it is
separated from all heterogeneous matters; which are left in the upper
crucible, while it passes through the holes in its bottom, and forms a
mass in the lower.
The precaution of closing all the apertures of both crucibles is
necessary, on account of the volatility of this mineral: and that the
Antimony, when once melted, may not continue exposed to a great heat,
it is made to run down into a vessel surrounded with ashes only, and
by that means very little affected with heat; ashes being one of those
solid mediums that transmit least of it.
PROCESS II.
_The common Regulus of Antimony._
Reduce crude Antimony to powder. Mix it with three fourths of its
weight of white Tartar, and half its weight of refined Salt-petre,
both pulverized. Into a large crucible made red-hot in the fire,
throw a spoonful of your mixture, and cover it. There will be a very
considerable detonation. When it is over, throw in a second spoonful
of your mixture, and cover the crucible as before: this will produce a
second detonation. Go on thus, till you have thrown in all your mixture.
When the whole has thus fulminated, increase the fire so as to bring
the matter into fusion; that being done, take the crucible out of the
furnace, and immediately pour its contents into an iron cone heated and
greased with tallow. Strike the floor and the cone some gentle blows
with a hammer, to make the Regulus precipitate: and when the matter
is fixed and cold, invert the cone and turn it out. You will see it
consist of two distinct substances; the uppermost of which is a saline
scoria, and the undermost the reguline part. Strike this mass a blow
with a hammer, in the place where these substances join, and you will
by this means separate the scoria from the Regulus; the latter of which
will have the form of a metallic cone, on whose base you will observe
the signature of a bright star.
_OBSERVATIONS._
Antimony, though separated by a former fusion from the earthy and stony
parts of its ore, must nevertheless be still considered as an ore, on
account of the great quantity of Sulphur it contains, which mineralizes
the metalline part or Regulus. Therefore, if you desire to have this
Regulus pure, you must separate it from the Sulphur that is combined
with it. This may be done several ways. The method above proposed
is one of the readiest and easiest, though not altogether free from
inconveniencies, as we shall shew.
The Salt-petre in the mixture detonates by means of the Sulphur of
the Antimony, which it consumes, and from which it separates the
reguline part: but lest it should also consume some of the phlogiston
which gives the Regulus its metalline form, Tartar is added; because
it contains a great deal of inflammable matter, and so is capable
of furnishing enough for the detonation of the Nitre, or rather for
restoring to the metallic earth of the Antimony, the phlogiston that
may be consumed by the Nitre.
If we consider what passes in this operation we shall soon be convinced
that a great deal must be lost in it, and that we do not thereby obtain
near the whole of the Regulus that the Antimony is capable of yielding:
for, 1. the Regulus of Antimony being a volatile substance, much of it
must be dissipated during the detonation; and so much the more as the
detonation is frequently repeated, and continued for a considerable
time. The flowers that may be collected by presenting cold bodies to
the smoke that rises in the operation, and which may be reduced to a
Regulus by the addition of a phlogiston, sufficiently prove what is
here advanced.
2. All the Sulphur of the Antimony is not consumed by the Nitre on
this occasion; and moreover, the Acid of that part thereof which is
burnt, uniting with some of the Alkali produced by the deflagration
of the Nitre and Tartar, forms a Vitriolated Tartar, which meeting
with a sufficient quantity of phlogiston in the mixture produces new
Sulphur. Now this Sulphur, whether not consumed, or reproduced, in the
operation, combining with the Alkali forms a Liver of Sulphur; and that
dissolves part of the Regulus, which by this means remains confounded
with the scoria. The proof of this is, that, if the scoria be mixed
with filings of iron, and fused a second time, you will find at the
bottom of the crucible a button of Regulus, which it contained, and
which is separated therefrom by the interposition of the Iron. We shall
say more on this subject in the process for making the Martial Regulus,
which immediately follows this. If, instead of melting the scoria
with iron filings, we pulverize it, boil it in water, and then pour
an acid into that water; the liquor will instantly grow turbid, and a
Sulphureous Precipitate will fall, commonly called _the Golden Sulphur
of Antimony_; which is nothing else but common Sulphur still combined
with some particles of the Regulus; a new proof of what we advanced
concerning the production of Liver of Sulphur in this operation.
As Regulus of Antimony is of no great value, the loss sustained in
this process is seldom regarded. However, we shall have occasion, in
the sequel, to point out a method of obtaining this Regulus with less
disadvantage.
PROCESS III.
_Regulus of Antimony precipitated by Metals._
Put one part of small iron nails into a crucible, and set it amidst
burning coals, in a melting furnace. When the iron is thoroughly
red-hot, and begins to grow white, add thereto little by little, and at
several times, two parts of crude Antimony in powder. The Antimony will
immediately flow and unite with the Iron. When the Antimony is entirely
melted, add thereto, at several times, the fourth of its weight of
pulverized Nitre: a detonation will ensue, and the whole mixture will
be in fusion.
After you have kept the matter in this condition for some minutes, pour
it into an iron cone, first heated and tallowed. Strike the sides of
the cone with a hammer, that the Regulus may fall to the bottom; and,
when all is cold, separate it from the scoria by a blow with a hammer.
Melt this first Regulus again in another crucible, adding a fourth
part of its weight of crude Antimony. Keep the crucible close shut,
and give no more heat than is necessary to melt the matter. When it is
in perfect fusion, add to it at several times, as you did before, the
sixth part of its weight of pulverized Nitre; and, in half a quarter
of an hour after this, pour the whole into a cone as you did the first
time.
Lastly, melt your Regulus over again a third, or even a fourth time,
always adding a little Nitre, which will detonate as before. If after
all these fusions you pour the Regulus into an iron cone, you will find
it very beautiful, and the star well formed: it will be covered with a
semi-transparent, lemon-coloured scoria. This scoria is extremely acrid
and caustic.
_OBSERVATIONS._
Though Regulus of Antimony unites very readily with Sulphur, and is
always found combined therewith in the earth, we must not thence
conclude that it hath a greater affinity than other substances with
that mineral: on the contrary, all the metals, except Gold, have a
greater affinity than this Semi-metal with Sulphur. Hence it follows
that all the metals, except Gold, are capable of decomposing Antimony,
and separating the sulphureous part from the metalline; so that,
instead of employing Iron, as in our process, Copper, Lead, Tin, or
Silver, may be used, and a Regulus obtained by means thereof.
But as Iron is, of all the metallic substances, that which hath the
greatest affinity with Sulphur, it is on this occasion preferred to
the rest. And from hence two advantages arise: the first is, that the
operation is performed sooner and with greater ease: the second, that
the Regulus is purer, and contains less of the precipitating metal. For
it is a general rule, that, when one metallic substance is employed
to precipitate another, the precipitated substance is always a little
adulterated by the admixture of some particles of the precipitant. Now,
the greater affinity the precipitant hath with the matter united to
that which is to be precipitated, the less doth the precipitate retain
of the precipitant.
In this process the Iron melts very easily by means of the union it
contracts with the Sulphur; which, as we observed before, hath the
property of rendering this metal very fusible, though of itself the
most refractory of all.
The scoria found on the Regulus of the first fusion is a combination
of Iron with the sulphureous part of the Antimony. This scoria is
extremely hard, and not to be separated from the Regulus without some
trouble. The Nitre added, being alkalizated and united therewith,
renders it a little softer, and gives it the property of relenting in
the air. Any Alkaline Salt may be substituted for the Nitre.
The Nitre that is alkalizated in the operation, or the Alkali that is
added, procures moreover another advantage; namely, that, by uniting
with part of the Sulphur of the Antimony, it produces a Liver of
Sulphur, which dissolves the Iron, retains it, and hinders that which
is not yet combined with pure Sulphur from uniting so readily with the
Regulus as it otherwise would do.
Lastly, the addition of Nitre, or an Alkali, contributes greatly to
promote the fusion, to render it more perfect, and to procure a more
complete precipitation of the Regulus.
The second fusion which the Regulus is made to undergo is intended to
purify it from any mixture of Iron. When the fresh Antimony added on
that occasion comes to melt with the Regulus, the Sulphur contained
in the Antimony joins with the ferruginous parts in the Regulus; and
the Iron becoming lighter by this union is thrown up to the surface
of the matter. There it forms a sort of scoria, with which a good
deal of Antimony is mixed; the Regulus not being wholly precipitated,
because there is not Iron enough in the mixture for that purpose. The
Salt-petre added here produces the same effect as in the first fusion.
But if, on one hand, the Regulus precipitated in the first fusion be
purified, by this addition of fresh Antimony, from most of the Iron
with which it was alloyed; on the other hand, this same Regulus cannot
be kept from re-uniting with some sulphureous parts.
In order therefore to separate it entirely from these, it must be
melted over again once or twice more, and a little Nitre added each
time, to consume them by deflagration. But this cannot be done
without consuming also some of the very phlogiston which gives the
Regulus its metalline form: whence it comes to pass that part of the
Regulus is converted to a calx, which, by means of the alkalizated
Nitre, is turned into glass; and it is this glass which mixing with
the scoria gives it the yellow colour observed therein. This yellow
colour may also be in part produced by some ferruginous particles,
of which a small quantity always remains combined with the Regulus,
notwithstanding its former depuration by Antimony.
It is of no use to repeat the fusions of the Regulus oftener than
is above proposed, or to add fresh Nitre with a view to consume the
Sulphur it may still contain: for after the second fusion it contains
none at all, and retains only the phlogiston necessary to give it the
metalline form. So that, by prosecuting the matter further, you would
only calcine and destroy the Regulus to no manner of purpose.
From what hath been said it is plain that, even by this process,
we do not obtain all the Regulus which our Antimony is capable of
yielding; seeing part of it is destroyed by the fusions it must
necessarily undergo with Nitre, in order to its purification. We shall
give a process for obtaining from Antimony the greatest quantity of
Regulus it can possibly be made to yield, after we have treated of its
Calcination, which is in some sort the first step of that process.
PROCESS IV.
_The Calcination of Antimony._
Take an unglazed earthen vessel, wider at top than at bottom; put
into it two or three ounces of crude Antimony finely pulverized. Set
this vessel over a weak charcoal fire, and increase the heat till you
see the Antimony begin to smoke a little. Continue the fire in this
degree, and keep incessantly stirring the Antimony with the shank of a
tobacco-pipe all the while it is upon the fire.
The powder of Antimony, which, before calcination, was of a brilliant
colour inclining to black, will become dull, and look like an earth.
When it comes to have this appearance raise your fire till the vessel
be red-hot, and keep it up in this degree till the matter cease
entirely to smoke.
_OBSERVATIONS._
Antimony, as hath been already said, is a sort of ore consisting of a
metalline or reguline part mineralized by Sulphur.
The design of this calcination is, by the action of fire, to dissipate
the sulphureous part, which is the most volatile, in order to separate
it from the metalline part. It is evidently a real torrefaction; but
the operation is very difficult, and requires a good deal of attention;
for Antimony very easily melts, while at the same time it is necessary
to our success that it do not melt; because when the matter is in
fusion the Sulphur requires a much greater degree of heat to carry it
off. Now, as Regulus of Antimony itself is very volatile, a good deal
of it would be dissipated along with the Sulphur, if it were exposed to
the degree of heat necessary to carry off the Sulphur when the mass is
melted.
Therefore if it happen that the Antimony begin to melt during the
calcination, which is easily perceived by its running into clots, it
must be taken off the fire, and the clotted parts be again pulverized;
after which the calcination is to be prosecuted with a less degree of
heat.
When the Antimony has lost all its brightness, and is become like an
earth, it is time to augment the degree of heat, in order to complete
the calcination; because the last portions of the Sulphur are the
most difficult to raise. Moreover, the inconveniences just mentioned
are not now to be apprehended: for, as the great fusibility of the
reguline part is owing to the Sulphur, what remains, after you have
dissipated the greatest part of the Sulphur, is much less fusible; and,
as the redundant Sulphur of the Antimony cannot be driven off, without
dissipating at the same time a good deal of the phlogiston necessary
to metallize its Regulus, the matter that remains comes much nearer
to the nature of a calx, than to that of a metalline substance; and
consequently partakes of the nature of all metallic calces, which is to
be very fixed.
Antimony may also be calcined by mixing with that mineral an equal
quantity of charcoal-dust. As charcoal is incapable of fusion, it
prevents the Antimony from clotting, as well as from losing so much of
its metallizing phlogiston as it otherwise would: and hence it comes
to pass that the calx of Antimony, prepared in this manner, comes
nearer to the nature of a Regulus, than that which is prepared without
addition.
If you happen to raise the fire too much, in this calcination with
charcoal-dust, the calx will be partly reduced to a Regulus, by means
of the phlogiston which the charcoal furnishes; and then the Regulus
will be dissipated in vapours, especially as this calx, which comes
very near the nature of a Regulus, is not so fixed as that prepared
without addition. For this reason it always continues to smoke, even
when it contains no superfluous Sulphur: and therefore you must not
wait till it cease to smoke before you put an end to your calcination;
for you will lose a great deal of it in vapours. It is time to stop
when the vapours that rise from it, while it is moderately red, do not
smell of burning Sulphur.
PROCESS V.
_Calx of Antimony reduced to a Regulus._
Mix the calx of Antimony, which you intend to reduce, with an equal
quantity of black soap. This mixture will make a thin paste. Put it
little by little into a crucible, previously made red-hot amidst live
coals. Thus let the soap burn till it cease to emit any oily smoke.
Then cover the crucible; make the fire strong enough to melt the
matter, and you will hear it effervesce and boil. When this noise is
over let the crucible cool, and then break it: you will find in it a
beautiful scoria, marked with circles of several colours; and under
that a button of Regulus, which is not yet quite pure, and must be
purified in the following manner.
Pound this Regulus, and mix it with half its weight of an antimonial
calx as perfectly desulphurated as possible. Put it into a crucible,
and cover it: melt the whole, so that the surface of the melted matter
may be smooth and uniform. Let the crucible cool, and then break it:
you will find in it a beautiful button of very pure Regulus, covered
with a scoria having the appearance of an opaque glass, or a kind of
greyish enamel, moulded on the finely radiated surface of the Regulus.
_OBSERVATIONS._
Of all the metalline calces that of Antimony is most easily reduced.
Any matter that contains the phlogiston, even charcoal-dust alone, is
sufficient to procure it the form of a Regulus, without the addition of
any thing to facilitate its fusion; because this calx, which is not of
itself altogether refractory, becomes still more fusible as it combines
with the phlogiston, and approaches to the reguline state.
Though all inflammable matters are capable of procuring the reduction
of the calx of Antimony, yet there are some with which the operation
succeeds better, and produces a greater quantity of Regulus, than it
does with others. Fatty matters, joined with Alkalis, are those which
answer best in this reduction, as they do in most others. The black
flux, for instance, is very proper for this purpose: but Mr. Geoffroy,
who made many experiments on Antimony, found by repeated trials that
black soap is still fitter for it, and that a greater quantity of
Regulus was obtained by its means, than by any other reducing flux
whatever. The process here given is taken from one of the Memoirs on
this subject, which he laid before the Academy of Sciences.
Black soap is made of the lye of a Fixed Alkali, such as potash
for instance, with quick-lime, incorporated by boiling with oil of
lint-seed, rape-seed, or hemp-seed, and sometimes also with animal fat.
The oily matters, contained in this reducing flux, are first burnt and
charred to a coal in the crucible. As soon as they are brought to this
state, the crucible is covered, and the fire is increased, till the
matters melt. At that instant the reduction begins to take place; and
the bubbling noise observed is an effect thereof.
The Regulus obtained by this first fusion is not yet very pure,
being adulterated with the mixture of some unmetallic earth that was
contained in the Antimony, and with a portion of the calcarious earth
of the soap.
Mr. Geoffroy found that his Regulus was contaminated with this
substance, by putting it into water: for on that occasion he observed
a very brisk ebullition about the reguline buttons, which sometimes
lasted above four and twenty hours; and on examining them with a glass,
he discovered some little holes, imperceptible to the naked eye,
through which the water entered, to unite with the lime retained in the
internal parts of the Regulus, which having been recalcined in the
operation required to be slaked.
This Regulus may be purified by simple fusion, without any additament,
because the particles of lime, being lighter than those of the Regulus,
will be thrown up to the surface, on which they will form a sort of
scoria. But Mr. Geoffroy took notice that, in this case, the surface
of the Regulus is never very neat; that it is always sullied with a
very adhesive scoria, and that no star is formed upon it. Besides,
the Regulus must be kept a long while in very thin fusion, that the
heterogeneous matters, which hinder the perfect re-union of its parts,
may have time to rise to the surface by their lightness. But the longer
the Regulus is kept in fusion, the more of it evaporates, because of
its volatility. He was therefore obliged to have recourse to other
means.
We have in the process described the method which succeeded best with
Mr. Geoffroy. It consists in melting the Regulus over again, with the
addition of a little fresh calx of Antimony thoroughly freed from
its Sulphur. This calx being in its nature easily vitrifiable, and
combining with the earthy parts that deprave the Regulus, and which
cannot be vitrified without addition, scorifies these matters, and with
them forms the opaque glass, or kind of enamel which is found over the
Regulus purified in this manner.
The star on that part of the Regulus of Antimony, which was contiguous
to the scoria, is a mark of its purity, and a proof that the operation
was well performed. This star is nothing but a particular disposition
of the parts of the Antimony, which have the property of running
naturally into facets and needles. The perfect fusion, both of the
Regulus and the scoria that covers it, leaves the parts of the Regulus
at liberty to range themselves in this order. This disposition appears
not only on the upper surface of the Regulus, but, if you break the
button, you find the same in its internal parts. There are some round
pyrites whose insides have nearly the same appearance, and seem to
consist of rays issuing from a common center.
The quantity of Regulus obtained by Mr. Geoffroy's process is more than
double of what is procured in the common way, which yields but about
four ounces in the pound; whereas this gives from eight to ten ounces.
When Antimony is calcined with charcoal-dust, what remains after the
dissipation of all the Sulphur is not, properly speaking, a calx of
Antimony; but a sort of Regulus quite formed, and differing from the
common Regulus only in that its parts are disunited, and not collected
into a mass. For if this pretended calx of Antimony be melted, it
directly coalesces into a Regulus, without the addition of any
inflammable matter fit to procure its reduction. Indeed less Regulus is
obtained by this means than when a reductive is added: but nevertheless
this experiment still proves what I advanced; seeing Regulus of
Antimony cannot be melted without losing more or less thereof, either
because some of it is dissipated in vapours, or because part of it
loses its phlogiston in the fusion, and so is converted into a calx.
PROCESS VI.
_Antimony calcined with Nitre. Liver of Antimony. Crocus Metallorum._
Pulverize and mix perfectly together equal parts of Nitre and Antimony:
put the mixture into an iron mortar, and cover it with a tile, which
however must not shut it quite close. With a live coal set fire to the
matter in the mortar, and immediately withdraw it. The mixture will
flame, with great detonation; which being over, and the mortar cooled,
invert it, and strike its bottom to make all the matter fall out. Then,
by a blow with a hammer, separate the scoria from the shining part,
which is the _Liver of Antimony_.
_OBSERVATIONS._
In this operation the Nitre takes fire and detonates with the Sulphur
of the Antimony; and nothing remains but the metallic earth of the
mineral, which, meeting with no substance to restore its phlogiston,
cannot take the form of a Regulus; but, being combined with a large
quantity of fused saline matters, begins itself to flow, and forms a
sort of vitrification; which, however, is not a complete one, because
the matters do not continue long enough in fusion, but cool too soon.
This preparation of Antimony is a violent Emetic. It is used to make
Emetic Wine and Tartar Emetic: it is also given in substance to horses.
The saline matters found after the operation in the form of a scoria,
or perhaps confounded with the Liver of Antimony, are combinations
of Fixed Nitre, partly with the Acid of the burnt Sulphur, forming a
Neutral Salt of the same kind as Vitriolated Tartar, and partly with
some unburnt Sulphur, forming a sort of Liver of Sulphur that contains
a little Regulus. It is usual to pulverize this Liver of Antimony and
wash it with water, in order to dissolve and carry off all the Salts.
When thus pulverized and washed it is called _Crocus Metallorum_. If
Liver of Antimony be melted with any inflammable matter, it will be
reduced to a Regulus; because it is nothing but a metalline calx half
vitrified.
PROCESS VII.
_Another Calcination of Antimony with Nitre. Diaphoretic Antimony._
Materia Perlata. Clyssus _of Antimony_.
Mix one part of Antimony with three parts of Nitre; project this
mixture by spoonfuls into a crucible kept red-hot in a furnace. Each
projection will be attended with a detonation. Continue doing this till
you have used all your mixture: then raise the fire, and keep it up
for two hours; after which throw your matter into a pan full of hot
water. Let it lie steeping in water kept hot for a whole day. Then pour
off the liquor: wash the white powder you find at bottom in warm water;
and repeat the ablutions till the powder become insipid. Dry it, and
you have _Diaphoretic Antimony_.
_OBSERVATIONS._
This operation differs from the preceding one, in respect of the
quantity of Nitre deflagrated with the Antimony. In the former we added
one part only of Nitre to one part of Antimony; but in this three parts
of Nitre are put to one of the mineral; and the calx resulting from
this mixture is of course very different from the other.
In the first place, Liver of Antimony hath a reddish colour; whereas
Diaphoretic Antimony is very white. Secondly, Liver of Antimony is in a
manner half vitrified; Diaphoretic Antimony is, on the contrary, in the
form of a powder, the parts of which have no connection together.
The reason of these differences will easily appear, if we consider,
that, Liver of Antimony being the result of calcination with one part
of the Nitre only, which is not sufficient to consume all the Sulphur
of the mineral, what remains after the detonation is not entirely
deprived of its phlogiston; from whence arise the colour it retains and
the ease with which it flows in the fire: but that, when three parts of
Nitre are added instead of one, this quantity is not only sufficient to
consume all the Sulphur and the phlogiston of the Antimony, but even
more than enough; seeing that, after the operation, some Nitre is still
found undecomposed.
The calx of Antimony, prepared by calcining it with three parts of
Nitre, is therefore deprived of all its phlogiston. This is the cause
of its whiteness, and the reason why it is not half vitrified by
the operation, as Liver of Antimony is: for we know that the more a
metallic calx is deprived of its phlogiston, the less fusible and
the less vitrifiable it is. This calx of Antimony bears the name of
_Diaphoretic Antimony_, or _Diaphoretic Mineral_: because, being
neither emetic nor purgative, it is thought to have the virtue of
promoting perspiration.
Antimony may be calcined with various proportions of Nitre, between
that used to make Liver of Antimony, and this with which Diaphoretic
Antimony is prepared; and from these calcinations will result calces
possessed of properties both chymical and medical, of an intermediate
nature between the extremes of those two preparations. The nearer
the proportion of Nitre comes to that employed in preparing Liver of
Antimony, the more will the resulting calx resemble that preparation;
and in the same manner, a calx prepared with a greater proportion of
Nitre will so much the more resemble Diaphoretic Antimony, as the
proportion of Nitre used comes nearer three parts of Nitre for one of
Antimony.
It is not necessary that Antimony in substance be employed to make the
Diaphoretic Mineral: you may, if you please, make use of its Regulus.
But as the Regulus contains no Sulphur, nor any more phlogiston than
is requisite to secure its metalline form, it is needless to put three
parts of Nitre to one of Regulus; an equal quantity thereof being
sufficient.
The matter is projected by spoonfuls, to the end that, by gradual and
repeated detonations, the Antimony may be more perfectly calcined:
it is also with a view to destroy entirely the small remainder of
phlogiston, which may have escaped the action of the Nitre, that the
matter is kept red-hot in the crucible for two hours.
The whole is afterwards thrown into hot water, and left steeping
therein for several hours, with design to give the water time to
dissolve all the saline matters that are mixed with the Diaphoretic
Calx. When crude Antimony is used in making this preparation, these
saline matters are, 1. an Alkalizated Nitre; 2. a Neutral Salt formed
by the union of the Acid of Sulphur with part of that Alkali, as in the
preparation of Liver of Antimony; 3. a portion of undecomposed Nitre.
The water in which the Diaphoretic is washed takes up moreover a
portion of the calx of Antimony, which is exceeding finely attenuated,
and continues united with the fixed Nitre, and suspended therewith in
the liquor. This matter is to be separated from the Fixed Nitre, by
mixing the water wherein it is dissolved with an Acid, which unites
with the Alkali, and precipitates this matter in the form of a white
powder, to which the name of _Materia Perlata_ hath been given.
Because it is precipitated in the same manner as the Golden Sulphur of
Antimony, and, like that, is found in the water with which the saline
matters are washed out, after the detonation of Nitre with Antimony,
some Chymists have given it, though very improperly, the name of the
_Fixed Sulphur of Antimony_.
This matter is a true Calx of Antimony, and differs from Diaphoretic
Antimony in nothing but its being still more perfectly calcined. It
is so indeed to such a degree that it is impossible to restore its
metalline form, or reduce it to a Regulus, by the addition of an
inflammable matter. Diaphoretic Antimony, on the contrary, may be
re-metallized, by supplying it with phlogiston: but it must be observed
that, in whatever manner you go about this, you will obtain a much
smaller quantity of Regulus, than when you use a Calx of Antimony
prepared with a smaller quantity of Nitre.
If you attempt to reduce either Liver of Antimony or Diaphoretic
Antimony, great care must be taken to wash them thoroughly, in order
to free them from every thing saline: for, without this precaution,
the Acid of the Sulphur, having, as was observed, formed a Neutral
Salt with the Alkali of the Nitre, will combine with the inflammable
matter added to revivify the calx of Antimony and reproduce a Sulphur;
which, uniting afterwards with the same Alkali, will produce a Liver
of Sulphur, that will dissolve part of the Regulus, hinder its
precipitation, and greatly lessen the quantity which might otherwise be
expected.
A particular sort of Diaphoretic Antimony is sometimes prepared for
Medical uses, which hath a purgative quality: it is not washed at all,
and is therefore called _Unwashed Diaphoretic Mineral_.
Diaphoretic Antimony may also be prepared in close vessels, by means
of which the vapours that rise during the operation are retained.
For this purpose a tubulated retort is employed, having a series of
adopters fitted to it. The retort is placed in a furnace, and heated
till its bottom become red: then a very small quantity of the mixture,
for making Diaphoretic Antimony, is introduced through the tube in
the upper part of the retort, and the tube immediately stopped. A
detonation ensues, and the vapours expand themselves into the adopters,
where they condense. This is repeated till the intended quantity of
matter be used. After the operation some white flowers are found
sublimed in the neck of the retort, and a small quantity of liquor in
the recipients. This liquor is acid. It consists of some of the Acid
of the Nitre, which the Acid of the Sulphur hath expelled from its
basis, and also a little of the Acid of the Sulphur carried up by the
heat before it could combine with the basis of the Nitre. This liquor
is called _Clyssus of Antimony_. The name of _Clyssus_ is given to all
liquors in general that are prepared by this method.
The white flowers found in the neck of the retort are flowers of
Antimony; that is, a calx of Antimony forced up by the heat, and by the
impetus of the detonation. These flowers may be reduced to a Regulus.
What remains in the retort is the same with the matter that remains
in the crucible, wherein the mixture of Nitre and Antimony for making
Diaphoretic Antimony hath been deflagrated.
Neither Diaphoretic Antimony nor the Pearly matter are soluble in any
Acid.
PROCESS VIII.
_Calx of Antimony Vitrified._
Take any quantity you please of calx of Antimony, made without
addition; put it into a good crucible, which set in a melting furnace:
kindle the fire gradually, and leave the crucible uncovered at the
beginning.
A quarter of an hour after the matter is red-hot, cover the crucible,
and excite the fire vigorously till the calx melt. You may know when it
is thoroughly melted, by dipping into the crucible an iron wire, to the
end of which a little knob of glass will adhere, if the matter be in
perfect fusion. Keep it in fusion for a quarter of an hour, or rather
longer if your crucible can bear it. Then take it out of the furnace,
and immediately pour out the melted matter on a smooth stone, made very
hot for the purpose: it will presently fix into a yellow Glass.
_OBSERVATIONS._
All the calces of Antimony, when exposed to a violent fire, are
converted into Glass; but not all with the same facility. In general,
the more of their phlogiston they have lost in the calcination, the
more difficult is their vitrification. This causes also a difference in
the colour of the Glass; which will be of so much a deeper yellow, and
the nearer to a red, the less the Antimony was calcined.
It frequently happens, when we employ a calx of Antimony which is not
sufficiently deprived of its phlogiston, that we find in the crucible a
button of Regulus, which, being heavier than the Glass, always lies at
the bottom. With a view to avoid this inconvenience, and to dissipate
completely the excess of phlogiston that may still be left in the calx
of Antimony, we direct the crucible to be left uncovered for some time,
at the beginning of the operation. If, notwithstanding this precaution,
any Regulus be still found at the bottom of the crucible, and you
resolve to vitrify it, the crucible must be returned to the furnace,
and the fusion continued; by which means the Regulus will at last be
converted into Glass.
If, on the contrary, you meet with any difficulty in effecting the
vitrification, on account of your having employed a calx that hath lost
too much of its phlogiston, such as Diaphoretic Antimony, or the Pearly
matter, the fusion may be greatly facilitated by throwing into the
crucible a little crude Antimony.
Glass of Antimony is a most violent emetic. This Glass, as well as
Liver of Antimony, is employed in preparing Emetic Wine and Emetic
Tartar.
It may be resuscitated, like the calces of Antimony, into a Regulus,
by re-uniting it with a phlogiston. For this purpose it must be
finely pulverized, thoroughly mixed with some black flux, and melted
in a covered crucible. This Glass, as well as that of Lead, hath the
property of greatly promoting the vitrification of matters that are to
be scorified.
PROCESS IX.
_Kermes Mineral._
Break any quantity you will of Hungarian Antimony into little bits:
put it into a good earthen coffee-pot: pour on it twice its weight of
rain-water, and a fourth part of its weight of well filtered liquor
of Nitre fixed by charcoal. Boil the whole briskly for two hours, and
then filter the liquor. As it cools it will acquire a red colour, grow
turbid, and leave a red powder on the filter.
Return your Antimony into the coffee-pot. Pour on it as much rain-water
as before, and three fourths of the former quantity of the liquor of
Fixed Nitre. Boil it again for two hours, and then filter the liquor.
It will again deposite a red sediment. Return your Antimony into the
coffee-pot: pour on it the same quantity of rain-water, and half the
first quantity of the liquor of Fixed Nitre. Boil it again for two
hours, and then filter the liquor as formerly. Wash all these sediments
with warm water, till they become insipid; then dry them, and you have
the _Kermes Mineral_.
_OBSERVATIONS._
If you recollect what we said concerning the property which Fixed
Alkalis possess of uniting with Sulphur, both by fusion, and, when
those Salts are resolved into a liquor, by boiling, and of forming
therewith a Liver of Sulphur, which dissolves all metalline substances,
you will readily comprehend the nature of this Kermes.
Antimony consists of a sulphureous and a reguline part. Therefore,
if this mineral be boiled in a solution of a Fixed Alkali, such as
Nitre fixed by charcoal, the Alkali will dissolve the Sulphur of the
Antimony, and form therewith a Liver of Sulphur, which, in its turn,
will dissolve the reguline part. Now, Kermes Mineral, prepared as above
directed, is no other than a Liver of Sulphur combined with a certain
quantity of Regulus of Antimony.
Mr. Geoffroy hath set this truth in the clearest light, by his
accurate analysis of the Kermes Mineral. The experiments he made on
that subject are circumstantially related in several Memoirs printed
in the volumes of the Academy for 1734 and 1735. By combining Acids
with the Kermes he demonstrated, 1. the existence of Sulphur in this
compound; having separated from it a burning Sulphur, which cannot
be mistaken for any other than the Sulphur of Antimony. In order to
obtain this Sulphur pure, an Acid must be employed that will not only
absorb the Alkali, but also perfectly dissolve the reguline part that
might otherwise remain united with the Sulphur. _Aqua regia_ was the
Acid which succeeded best with Mr. Geoffroy. 2. He also proved that
there is a Fixed Alkali in the composition of the Kermes; seeing the
Acids with which he precipitated the Sulphur became Neutral Salts, and
just such as those very Acids combined with a Fixed Alkali would have
constituted: that is, the Vitriolic Acid produced a _Sal de duobus_;
the Nitrous Acid a regenerated Nitre; and the Marine Acid a regenerated
Sea-salt. 3. Mr. Geoffroy demonstrated the reguline part of Antimony
to be an ingredient in the Kermes; having procured therefrom an actual
Regulus of Antimony, by fusing it with the black flux.
In preparing the Kermes it is necessary to renew the liquor from time
to time, as above directed; because, when it is once impregnated with
Kermes to a certain degree, it can take up no more; and consequently
the same liquor cannot operate again on the Antimony. Experience hath
shewn, that, if the doses above prescribed be applied, the liquor will
after two hours boiling be sufficiently saturated with Kermes.
If the liquor in which the Kermes is dissolved be filtered while it
is very hot, and almost boiling, it leaves nothing on the filter; the
Kermes passing through with it: but as it cools it grows turbid, and
gradually deposites the Kermes. Therefore it ought not to be filtered
till it be cold; or, if it be filtered while it is boiling hot, in
order to separate from it some coarse particles of Antimony not yet
converted into Kermes, it must be filtered a second time when it is
cold, in order to get the Kermes.
Though in the method usually practised for making Kermes, the Antimony
is boiled only thrice, yet it does not follow that more Kermes may not
be obtained from it, or that but little more would be obtained by a
fourth and fifth boiling; on the contrary, it would yield considerably
more. Mr. Geoffroy observed, that he got more Kermes by the second
boiling than by the first, and still more by the third than by the
second; and that the yield goes on increasing in this manner to a very
great number of times, which he hath not determined. This increased
effect arises from hence, that by multiplying the frictions of the
little bits of Antimony against each other, new surfaces are exposed to
the action of the Alkaline liquor, and furnish it with more Sulphur;
while the addition of this sulphur renders the hepar more active and
more penetrating; or, if you please, produces a new hepar every time
the matters are boiled. When the Alkaline liquor is once saturated
with Kermes, it ceases to act, and forms no new hepar; but it does
not follow that its virtue is quite exhausted. To restore its ability
of acting as well as at first, or nearly so, you need only let it
cool, and deposite the Kermes dissolved in it. We owe this singular
observation also to Mr. Geoffroy: he had the patience to go through no
less than threescore and ten boilings with the same liquor, without
adding any thing but rain water, to supply the place of what was
dissipated by evaporation: and he always obtained a pretty considerable
quantity of Kermes by each boiling, for the reason given above.
Boiling is not the only means of making Kermes. Mr. Geoffroy found the
way of making it by fusion. For this purpose you must mix accurately
one part of very pure Fixed Alkali, dried and pulverized, with two
parts of Hungarian Antimony also pulverized, and melt the mixture.
Mr. Geoffroy made use of a retort. When the mass is melted, it must
again be pulverized, while it is still hot, and then put into, and
kept in, boiling hot water for an hour or two; after which the liquor,
now become saline and antimonial, must be filtered into another vessel
filled with boiling water. Every ounce of Antimony treated in this
manner yields, by thrice boiling the melted mass, from six drams to
six drams and a half of Kermes; which differs from the Kermes made by
boiling, only in that it is not quite so soft to the touch, having in
every other respect the same qualities.
As Liver of Sulphur is made two different ways, to wit, by boiling and
by fusion, and as the Kermes is nothing but a Liver of Sulphur in which
the reguline part is dissolved; it follows that Kermes may be made by
fusion as well as by boiling. It is necessary to pulverize the melted
mass, and to steep it in boiling hot water for an hour or two, that the
water may dissolve and divide it sufficiently to make the Kermes fine
and beautiful.
With the same view, that is, to make it finer and more perfect, Mr.
Geoffroy orders the water saturated with the Kermes made by fusion,
to be received, when filtered, in a vessel full of other boiling hot
water. He observed, that when the liquor impregnated with Kermes cools
too fast, the Kermes that precipitates is much coarser. The warm
solution of Kermes is diffused through the boiling-hot water into which
it is filtered, and is thereby enabled to retain its heat so much the
longer.
From what hath been said on the nature of Kermes, it plainly appears
that there must be a great resemblance between it and the Golden
Sulphur of Antimony, obtained from the scoria, either of plain Regulus
of Antimony, or of the Liver of Antimony; this Golden Sulphur being
no other than a portion of the Antimony combined with the Nitre
alkalizated during the operation.
Yet there is a difference in the manner of precipitating these two
compounds: for the Kermes precipitates spontaneously, on the bare
cooling of the water in which it is dissolved; whereas an Acid is
employed to precipitate the Golden Sulphur suspended in the water, with
which the scoria of the plain Regulus of Antimony, or that of Liver of
Antimony, hath been washed. This gives some ground to suspect that the
reguline part is not so intimately united with the Liver of Sulphur in
the Kermes, as in the scoriæ from which the Golden Sulphur is obtained.
PROCESS X.
_Regulus of Antimony dissolved in the Mineral Acids._
Compound an _aqua regis_ by mixing together four measures of Spirit of
Nitre, and one measure of Spirit of Salt: on a sand-bath moderately
heated place a matrass, into which pour sixteen times as much of this
_aqua regis_ as you have Regulus to dissolve. Break your Regulus
into little bits; and throw them successively one after another into
the matrass, observing not to add a new one till that put in before
is entirely dissolved: continue this till your Regulus be all used.
By degrees, as the dissolution advances, the liquor will acquire a
beautiful golden colour; which, however, will insensibly disappear, as
the white fumes that continually ascend from it evaporate.
_OBSERVATIONS._
Regulus of Antimony is one of those metalline substances that dissolve
with the greatest difficulty. Not but that most of the Acids attack
and corrode it; but they do not make a clear, limpid solution thereof:
they in some sort only calcine it, and this semi-metal, as fast as
it dissolves, precipitates of its own accord in the form of a white
magistery. In order to effect a complete dissolution thereof, it is
necessary to employ an _aqua regis_ compounded as directed, and in
the dose prescribed in the process, which is wholly taken from Mr.
Geoffroy's Memoirs on Antimony mentioned above.
If, instead of the Regulus, small bits of crude Antimony be thrown into
the _aqua regis_, the Acid will attack and dissolve the reguline part,
and so separate it from the sulphureous part which it will not touch.
When the dissolution is finished, the particles of Sulphur being now
become lighter, because no longer united with the metalline part, will
float upon the liquor. Being collected they form a true Sulphur, which
seems no way different from common brimstone. This operation, you see,
is a sort of Parting Process.
The Vitriolic Acid, whether concentrated or much weakened with water,
does not act when cold either on Antimony or on its Regulus. This Acid
only dims the splendour of the facets of the Regulus; but if one part
of exceeding pure Regulus of Antimony be put into a retort, and four
parts of clear concentrated Oil of Vitriol poured on it, as soon as the
Acid is heated it turns brown, and emits a most suffocating smell of
Sulphur, which increases as the Regulus is penetrated and corroded by
the Acid.
On raising the fire, there separates from it a matter that seems
mucilaginous; and when the Acid hath boiled some time, the Regulus is
converted into a white saline mass, as Mercury is in the preparation of
Turbith mineral. At the same time a little Sulphur sublimes into the
neck of the retort. At last all the Oil of Vitriol passes over into the
receiver, and leaves the Regulus in a white, spungy, saline mass in the
retort. When the fire is out, the vessels unluted, and the receiver
separated from the retort, there rises a white vapour like that of the
smoking liquor of Libavius.
The saline mass left in the retort, after the operation, is found
increased to near double its weight: this increased weight is owing to
the Acid that hath united with the Regulus.
This combination of the Vitriolic Acid with the Regulus of Antimony
is excessively caustic, and cannot, for that reason, be administered
internally.
The purest Spirit of Salt hath no sensible effect either on Antimony
or its Regulus: but if Antimony be coarsely pounded, it separates
therefrom, though slowly, some light, sulphureous flakes.
The action of Spirit of Nitre on this metallic substance is more
perceptible: by little and little it attacks the plates of the
Antimony, which discharge a great number of air-bubbles. As the
dissolution advances, the Acid acquires a greenish colour inclining to
blue; and if there be not too much of it, it will be almost entirely
imbibed by the Antimony, penetrate between its _laminæ_, and exfoliate
them in the direction of the needles that compose them. If there be
too much of the Acid, that is, if it rise above the Antimony, it will
destroy these plates, and reduce them to a white powder.
But when the Acid is imbibed slowly, we discover between the swelled
_laminæ_ little saline transparent crystals, that vegetate much in the
same manner as those of the pyrites, in which small crystals of Vitriol
are frequently observed, whose figures are not very well determined.
These little crystals between the Antimonial plates are intermixed with
yellow particles, which being carefully separated burn like common
Sulphur.
All these useful observations, concerning the action of the Acids on
Antimony and its Regulus, we owe likewise to Mr. Geoffroy; who advises
the collecting a quantity of these little crystals in time; because
they disappear soon after they are formed, being probably covered by
the white powder, or magistery, which is continually produced as fast
as the Nitrous Acid disunites and separates the needle-like fibres of
the Antimony.
Mr. Geoffroy observed the same sort of crystals on the Regulus of
Antimony, when substituted for crude Antimony in this experiment;
but it requires a great deal of care to separate these crystals;
for as soon as the air comes into contact with them they lose their
transparency; and if you wait till the Regulus be in some measure
converted into a magistery, they are not then to be distinguished.
In order therefore to have a good view of these crystals, the Regulus
must be broken to pieces; these pieces put in a glass bason, and Spirit
of Nitre poured on them to half their heighth, but not to cover them.
This Acid penetrates them, exfoliates them in white scales; and on the
surface of these scales the crystals shoot of a dead white colour. In
two or three days time these crystals vegetate and grow in the form
of cauli-flowers: they must then be gathered, to prevent their being
confounded in the white magistery which continues to be produced,
and would not suffer them to be distinguished. If you attempt to
dissolve the reguline part of Antimony by an _aqua regis_ compounded
in different proportions, and applied in a different dose from what
is prescribed in the process, the Regulus of Antimony will only be
calcined, as it is by the other Acids, and will precipitate in the form
of a white magistery as fast as it dissolves, so that no part thereof
will remain united with the solvent. The proof of this is, that if an
alkaline liquor be poured, even to the point of saturation, upon the
_aqua regis_ that hath thus dropt the Antimony, no new precipitate will
be deposited.
PROCESS XI.
_Regulus of Antimony combined with the Acid of Sea-salt. Butter of
Antimony. Cinabar of Antimony._
Pulverize and mix thoroughly six parts of Regulus of Antimony, and
sixteen parts of Corrosive Sublimate. Put this mixture into a glass
retort that hath a wide short neck, and let one half of its body at
least be left empty. Set it in a reverberatory furnace, and having
fitted a recipient thereto, and luted the joint, make a very small fire
at first, to heat it slowly. Increase it afterwards by degrees, till
you see a liquor ascend from the retort that grows thick as it cools.
Keep up the fire to this degree as long as you see any of this matter
come over.
When no more rises with this degree of fire, unlute your vessels, take
off the receiver, and in its place substitute another filled with
water. Then increase your fire by degrees till the retort be red-hot.
Some running Mercury will fall into the water, which you may dry and
keep for use; it being very pure.
_OBSERVATIONS._
In our observations on the preceding process, we took notice that the
purest Marine Acid, in the form of a liquor, will not dissolve the
reguline part of Antimony. Here this very Acid combined with Mercury,
and applied in a dry form to the Regulus of Antimony, quits the Mercury
with which it was united, in order to join this very Regulus, as having
a greater affinity therewith. This operation is a further proof of what
we advanced on the subject of Mercury; to wit, that several metallic
substances, which are not soluble by certain Acids when in a fluid
state, may be dissolved by those Acids when most highly concentrated;
as they are when combined with any other substance in a dry form, and
are separated from it by the force of fire. Their efficacy is also
further promoted by their being reduced, on this occasion, into subtile
vapours.
The Marine Acid combined with the reguline part of Antimony doth not
form a hard, solid compound; but a kind of soft substance, that melts
in a very gentle heat, and also becomes fixed by the least cold, much
in the same manner as butter; and from this property it hath its name.
Soon after mixing the Regulus with the Corrosive Sublimate, the matter
sometimes grows considerably hot: this is occasioned by the Marine
Acid's beginning to act on the reguline part, and to desert its Mercury.
The Butter of Antimony rises with a very moderate heat; because the
Acid of Sea salt hath the property of volatilizing, and carrying up
along with it, the metallic substances with which it is combined: and
for this reason a very gentle heat only is required at the beginning of
the operation.
It is absolutely necessary that the neck of the retort be wide and
short: for otherwise if the Butter of Antimony should fix and be
accumulated therein, it might stop up the passage entirely, and
occasion the bursting of the vessels. By this operation we obtain eight
parts and three quarters of fine Butter of Antimony, and ten parts of
running Mercury; there being left in the retort one part and a half of
a rarefied matter, black, white, and red. This is probably the most
earthy and most impure part of the Regulus of Antimony.
It is of the utmost consequence to the operator that he avoid with the
greatest care the vapours that issue from the vessels, because they are
extremely noxious, and may occasion mortal disorders. The Butter of
Antimony is a most violent Corrosive and Caustic.
When all the Butter is risen, the receiver is shifted in order to
receive the Mercury; which, being disengaged from the Acid that gave
it a saline form, appears in its natural form of Quick-silver: but it
requires a much greater degree of heat than the Butter of Antimony to
raise it by distillation.
If crude Antimony, instead of Regulus of Antimony, be mixed with
Corrosive Sublimate, a Butter of Antimony will be obtained in the same
manner; but, instead of having a running Mercury after the Butter, you
will find a Cinabar sublimed into the neck and upper concavity of the
retort.
The reason of this difference is easily conceived: for when the
Regulus is used, the Mercury being deserted by its Acid finds no other
substance to unite with, and so rises in the form of Quick-silver; but
when crude Antimony is employed instead of its Regulus, as the reguline
part thereof cannot combine with the Acid without quitting its Sulphur,
so this Sulphur, being at liberty, unites with the Mercury, which is so
likewise, and therewith forms a Cinabar; which from its origin is named
_Cinabar of Antimony_. When you intend to make both Butter and Cinabar
of Antimony at the same time, six parts of Antimony must be mixed with
eight of Corrosive Sublimate; and care must be taken, while the Butter
is coming over, to warm the neck of the retort by holding some live
coals near it, with the precautions necessary to avoid breaking it.
This warmth makes the Butter melt and run into the receiver; whereas,
being thicker and of a much denser consistence than that made with the
Regulus, it would otherwise gather in the neck of the retort, choak it
entirely, and burst the vessel.
When the Butter is drawn from crude Antimony, more circumspection is
necessary to make it of a beautiful white colour, than when it is
obtained from the Regulus: for, if the fire be too strong during the
distillation, or if the receiver be not soon enough separated from the
neck of the retort, certain red sulphureous vapours, the fore-runners
of the Cinabar, will at last ascend, and mixing with the Butter give it
a brown colour.
In order to restore its beauty it must be put into a clean retort,
and rectified by distilling it over again with a gentle sand-heat.
By this rectification the Butter of Antimony becomes more fluid; and
by re-distilling it a second time you may give it the thinness and
fluidity of an oil.
After the operation there will be found in the receiver three parts and
three quarters of Butter of Antimony, and some small crystals adhering
to its inside, in the form of sprigs. When you break the retort there
exhales from it a sulphureous odour; and you will find in it seven
parts of Cinabar of Antimony, the greatest part of which is usually in
compact glebes, that are heavy, smooth, shining, blackish throughout
most of the mass, but in some places red: another part thereof appears
in shining needles, and the rest in powder.
When all the Butter of Antimony is come over, and you begin to see the
red vapours that predict the approaching ascent of the Cinabar, the
receiver containing the Butter must be removed, lest the colour of the
Butter should be spoiled by those sulphureous vapours. Another receiver
is usually fitted on, without luting; in which a small quantity of
running Mercury is sometimes found, when the operation is finished.
There remains, at the bottom of the retort, a fixed, shining,
crystalline, black mass, which may be reduced to a Regulus by the
common method.
Butter of Antimony may also be obtained from a mixture of Antimony with
any of the other preparations of Mercury in which the Acid of Sea-salt
is an ingredient; such as sweet Sublimate, the Mercurial Panacea, and
White Precipitate: but as none of these combinations contain so great
a proportion of that Acid as is in the Corrosive Sublimate, the Butter
obtained by their means is far from being so caustic and so fiery as
that which rises from a mixture of Antimony, or its Regulus, with
Corrosive Sublimate.
Silver precipitated by the Acid of Sea-salt, and ready to be melted
into a _Luna cornea_, being mixed with powdered Regulus of Antimony
yields likewise a Butter of Antimony.
If you propose to make it by this means, you must mingle one part of
the Regulus of Antimony in powder with two parts of the Precipitate;
put this mixture into a glass retort of such a size that it may fill
but one half thereof; set it in a furnace; apply a receiver; begin
with a gentle heat, which will make a clear liquor come over; and then
increase your fire by degrees. White vapours will rise and condense
into a liquid Butter; and in the mean time there will be a slight
ebullition in the receiver, attended with a little heat. Continue the
fire till nothing more will come over; then let your vessels cool and
unlute them.
You will find in the receiver an Oil or Butter of Antimony, partly
fluid and partly congealed, somewhat inclined to yellow, weighing an
eighth part more than the Regulus of Antimony made use of.
The inside of the retort will be carpeted over with small white
flowers, of a brilliant silver colour, and an acid taste; and in the
bottom of the retort will be found a hard, compact, ponderous mass,
difficult to break, yet falling of itself to a powder; its colour
externally grey, white, and blueish; internally black, and shining much
like Regulus of Antimony; having a saltish taste on its surface, and
weighing about a sixteenth less than the Precipitate of Silver employed
in the operation.
This experiment demonstrates that the Acid of Sea-salt hath a greater
affinity with Regulus of Antimony than with Silver.
The Butter of Antimony prepared by this method is somewhat less caustic
than that made with Corrosive Sublimate. It is called the _Lunar Butter
of Antimony_.
The effervescence that arises in the receiver is remarkable. Probably
the Acid of Sea-salt, though reduced into vapours when it ascends out
of the retort, is not yet perfectly combined with the reguline part
of the Antimony, which it nevertheless carries over with it, and the
union is completed in the receiver; which occasions the effervescence
observed.
The little white silvery flowers, adhering to the inside of the retort,
are flowers of Regulus of Antimony, which sublime towards the end of
the distillation.
The compact mass, found at the bottom of the retort, is no other than
the Silver separated from its Acid, and combined with a portion of the
Regulus of Antimony. The colours and the saltish taste of its surface
are occasioned by a remainder of the Marine Acid. This Silver is
rendered brittle and eager by the union it hath contracted with some of
the Regulus of Antimony.
It is easy to purify it, and restore its ductility, by separating it
from the Regulus of Antimony. There are several ways of doing this:
one of the most expeditious is to flux it with Nitre, which burns and
converts to a calx the semi-metal with which the Silver is adulterated.
PROCESS XII.
_Butter of Antimony decompounded by means of Water only. The_ Pulvis
Algaroth, _or_ Mercurius Vitæ. _The Philosophic Spirit of Vitriol._
Melt with a gentle heat as much Butter of Antimony as you please.
When it is melted, pour it into a large quantity of warm water. The
water will immediately grow turbid, but whitish, and let fall a great
quantity of white powder. When all the precipitate is settled, decant
the water: pour on fresh warm water; and having thus edulcorated it
by several ablutions, dry it, and you have the _Pulvis Algaroth_, or
_Mercurius Vitæ_.
_OBSERVATIONS._
In the preceding processes we observed that the Marine Acid will not
dissolve the reguline part of Antimony, unless it be very highly
concentrated, and more so than it can possibly be while in the form of
a liquor. Of this the experiment before us is a further proof. Whilst
the Marine Acid is so perfectly dephlegmated, as it is in Corrosive
Sublimate and Butter of Antimony, it remains combined with the reguline
part of Antimony; but if this combination be dissolved in water, the
moment the Acid is weakened by the interposition of the particles of
water, it becomes incapable of continuing united with the semi-metal
which it had before dissolved; deserts it, and lets it fall in the
form of a white powder.
The _Pulvis Algaroth_ is therefore no other than the reguline part of
Antimony, attenuated and divided by the union it had contracted with
the Acid of Sea-salt, and afterwards separated from that Acid by the
intervention of water alone. The proof is, that this powder retains
none of the properties of the Butter of Antimony: it is neither so
fusible nor so volatile; on the contrary, it is capable of sustaining a
very strong degree of fire, without subliming and without melting: it
may be reduced to a Regulus: it hath not now the same caustic nature:
it is only an emetic; which however is extremely violent, and on that
account is never prescribed by any prudent physician.
Another proof, that the Marine Acid is separated from the Regulus of
Antimony in the precipitation of the _Pulvis Algaroth_, is, that the
water in which this precipitation is made becomes acid, or a sort
of weak Spirit of Salt. If it be evaporated, and concentrated by
distillation, a very strong acid liquor may be obtained from it. This
Acid goes, very improperly, by the name of the _Philosophic Spirit of
Vitriol_; for it is rather a Spirit of Salt.
The _Pulvis Algaroth_, made with Butter of Antimony procured from the
Regulus, is whiter than that made with Butter of Antimony procured
from crude Antimony; probably because the latter always retains some
sulphureous particles.
Butter of Antimony exposed to the air attracts the moisture thereof,
and partly runs into a liquor; but, as fast as this liquor is
produced, it deposites a white sediment, which is an actual _Pulvis
Algaroth_. This also is very agreeable to what we advanced touching
the decomposition of Butter of Antimony by the addition of water. The
Butter attracts the moisture of the air, because the Acid it contains
is exceedingly concentrated; and this moisture produces the same effect
as water purposely added.
PROCESS XIII.
_Bezoar Mineral. The Bezoartic Spirit of Nitre._
Melt Butter of Antimony over warm ashes, and put it into a phial or
matrass. Gradually pour on it good Spirit of Nitre, till the matter
be entirely dissolved. This usually requires as much Spirit of Nitre
as there is Butter of Antimony. During the dissolution fumes will
rise, which must be carefully avoided. Pour your solution, which will
be clear and of a reddish colour, into a glass cucurbit, or a pan of
stone-ware: set it in a sand-bath, and evaporate to dryness with a
moderate heat. There will be left a white mass, weighing a fourth part
less than the whole quantity used, both of the Butter and the Spirit
of Nitre. Let it cool, and again pour on it as much Spirit of Nitre as
you used the first time. Place the vessel again in the sand-bath, and
evaporate the moisture as before. You will have a white mass that hath
neither gained nor lost in weight. On this pour, for the third time,
the same quantity of Spirit of Nitre as you did the first time. Again
evaporate the moisture to perfect dryness: then increase your fire,
and calcine the matter for half an hour. You will have a dry, friable,
light, white matter, of an agreeable acid taste; which will fall into
a coarse powder, and must be kept in a phial carefully stopt. This
is _Bezoar Mineral_: it is neither caustic nor emetic, and has only
a sudorific virtue. It obtained the name it bears, because, like the
animal Bezoar, it was imagined to have the property of resisting poison.
_OBSERVATIONS._
It is not surprising that the Nitrous Acid poured on Butter of Antimony
should dissolve it, and unite with it: for with the Marine Acid, which
makes a part of this combination, it forms an _aqua regis_, which we
know is the true solvent of the reguline part of Antimony. But in this
dissolution, and the changes it produces, there are some things very
remarkable and worthy of attention. 1. The Nitrous Acid, by uniting
with the Butter of Antimony, deprives it of its property of rising with
a very gentle heat, and makes it much more fixed: it can now be dried,
and suffer all its moisture to be evaporated; which is not to be done
with pure Butter of Antimony: for that, being exposed to a certain
degree of heat, instead of letting go its moisture and remaining dry,
rises wholly, without the least appearance of any separation of parts.
2. The Butter of Antimony, which, before its combination with the
Nitrous Acid, is a most violent Caustic and Corrosive, becomes so mild
after it, that it may not only be taken internally without danger, but
hath scarce any sensible operation.
The following considerations will lead us to a reasonable explanation
of these phenomena. 1. The Nitrous Acid, when combined with metallic
substances, doth not communicate to them the same volatility as they
acquire from the Marine Acid. Hence it follows, that, if the Nitrous
Acid be added to any combination of a metallic substance with the
Marine Acid, this new compound will be rendered less volatile, and
consequently more able, without rising in vapours, to bear a degree of
heat sufficient to carry off part of its Acid. This is the case with
Butter of Antimony, after Spirit of Nitre is mixed with it; especially
considering, 2. That the Nitrous Acid cannot unite with the reguline
part of the Butter of Antimony without weakening the connection between
it and the Marine Acid; whence it follows, that the combination of the
Nitrous Acid further facilitates the separation of the Marine Acid
from the Regulus. Now as soon as the Marine Acid quits the reguline
part, that part becomes more fixed, and consequently more capable of
enduring the degree of heat requisite to discharge all the adhering
Acid; and not only the Marine, but even the Nitrous also. It is not
therefore surprizing that, after the Antimony which remains combined
with the Nitrous Acid is dried, it should not possess that corrosive
power which it derives only from the Acids wherewith it is armed. In
order to free it more perfectly from all Acid, we order the fire to be
increased after the third desiccation; and the remainder of the Butter
of Antimony to be calcined for a full half-hour longer.
That the Marine Acid is separated from the reguline part of the Butter
of Antimony, by the desiccations it undergoes in converting it into
Bezoar, is proved by this, that, when these desiccations are performed
in close vessels, the liquor drawn off is a true _aqua regis_, known by
the name of the _Bezoartic Spirit of Nitre_.
It remains to be considered why the Bezoar mineral, though freed from
all acid, is not emetic; while the _Pulvis Algaroth_, which is likewise
the reguline part of the Butter of Antimony deprived of its Acid,
is such a violent emetic, and even to be dreaded for its remaining
causticity.
In order to discover the reason of this difference, it is proper to
observe that, when we say Bezoar mineral and the _Pulvis Algaroth_
contain no Acid, we must not be understood in too strict a sense: on
the contrary, there is reason to think that a certain quantity of Acid
still remains in each of them; which however is scarce worth notice,
in comparison of the quantity each contained at first. This being
allowed, it will not be hard to find the difference between these two
preparations of Antimony. The _Pulvis Algaroth_ is deprived of its
Acid by the addition of water alone, which only carries off all the
loose Acid it can take up, without making any change in the nature of
that which continues in combination with the reguline part. Now, as
the Marine Acid is not intimately united with the reguline part in
Butter of Antimony; as it still retains some of its properties, such as
attracting the moisture of the air, giving manifest tokens of its Acid
nature, &c.; and as the corrosive quality of this compound depends on
this last in particular; the small portion of Acid left in the _Pulvis
Algaroth_ will in some degree preserve its former character: and hence
comes the effect of this powder, which still retains a little of the
corrosive quality that belonged to the Butter of Antimony.
But this is not the case with the small remainder of Acid, which
possibly still continues united with the Bezoar mineral prepared as
here directed. This compound hath been exposed to a fire sufficient,
not only to dry it, but even to calcine it. Now fire is capable of
producing great changes in the texture of bodies. It must have forced
off from the Bezoar all the Acid that was not intimately combined
with it; and that part which it could not drive off, because of its
obstinate adhesion, it must have further united and combined more
closely with the metallic earth: for we see that fire greatly promotes
the action of solvents on the matters with which they are united.
With regard to the properly emetic quality of the _Pulvis Algaroth_,
it cannot be imputed to the combination of any Acid with that powder;
since we see that the most powerfully emetic preparations of Antimony,
_viz._ its Regulus and Glass, contain no Acid: it must therefore be
attributed to some cause different from that on which its corrosive
quality depends. This cause we shall easily find by attending to the
different manners in which the Marine Acid, when alone and in _aqua
regia_, operates on the reguline part of Antimony.
The Marine Acid alone dissolves the Regulus of Antimony, but with
great difficulty; nor doth it effect a complete dissolution thereof,
as is evident from what hath been already said: whereas the Marine
Acid, combined with the Nitrous Acid, and therewith forming an _aqua
regis_, as in the preparation of Bezoar, dissolves the reguline part
of Antimony completely and radically. Now, it is certain that, the
more efficaciously Acids operate on metallic substances, the more of
their phlogiston do they destroy; and we cannot but recollect that
the preparations of Antimony are so much the less emetic the less
phlogiston they contain, or the further they recede from the nature
of a Regulus, and the nearer they approach to that of Diaphoretic
Antimony: consequently it is plain how Bezoar mineral, which is a
sort of calx of Antimony entirely deprived of its phlogiston by the
intimate dissolution thereof made by the Acids of the _aqua regis_,
may be in no degree emetic; while the _Pulvis Algaroth_, being a true
Regulus of Antimony, on which the Marine Acid hath operated but very
superficially, and which still contains a great deal of phlogiston, is
a most violent emetic.
PROCESS XIV.
_Flowers of Antimony._
Take an unglazed earthen pot, having an aperture in its side, with a
stopple to shut it close. Set this pot in a furnace, the cavity whereof
it may fit as exactly as possible; and fill up with lute the space,
if any, left between the vessel and the furnace. Over this vessel fix
three aludels, with a blind-head at the top; and light a fire in the
furnace under the pot.
When the bottom of the pot is thoroughly red, throw into the lateral
aperture a small spoonful of powdered Antimony. Stir the matter
immediately with an iron spatula made a little bending, in order to
spread it over the bottom of the vessel, and then stop the hole. The
flowers will rise and adhere to the insides of the aludels. Keep up the
fire so that the bottom of the pot may always continue red; and, when
nothing more sublimes, put in a like quantity of Antimony, and operate
as before. In this manner go on subliming your Antimony, till you have
as many flowers as you want. Then let the fire go out; and when the
vessels are cold unlute them. You will find flowers adhering all round
the insides of the aludels and the head, which you may collect with a
feather.
_OBSERVATIONS._
Antimony is a volatile mineral, capable of being sublimed into flowers;
but this cannot be effected without occasioning a notable change
in its parts. The reguline and the sulphureous parts are not united
so intimately, or in the same proportion, in the flowers as in the
Antimony itself; and accordingly we find these flowers have a strong
emetic quality, which Antimony hath not. They are of divers colours;
which probably arises from their containing more or less Sulphur. Three
or four aludels are placed one over another, not only with a view to
provide a greater surface, to which the flowers may adhere, but also to
give them room enough to circulate, without which they might burst the
vessels.
If you introduce the nosle of a pair of bellows into the pot that
contains the Antimony, and blow upon it, the sublimation of the flowers
will be much sooner effected. This is a general rule with regard to all
matters that are to be sublimed or evaporated; the reason of which we
have already given.
It is proper that no interval be left between the furnace and the pot
containing the Antimony, lest the heat should be thereby communicated
to the aludels, on which the flowers fasten best when they are cold.
After the operation, there remains at the bottom of the pot a portion
of Antimony half calcined; which being pulverized, and thoroughly
calcined till it emit no fume, may be employed to make the Glass of
Antimony.
PROCESS XV.
_Regulus of Antimony converted into Flowers._
Pulverize your Regulus of Antimony: put the powder into an unglazed
earthen pot: three or four fingers breadth above the powder, fit into
the pot a little cover, made of the same earth, and having a small
hole in its middle, so that it may with ease be placed in the pot, and
taken out when there is occasion: cover the mouth of the pot with a
common lid; set it in a furnace, and kindle a fire under it sufficient
to make the bottom of the pot red, and to melt the Regulus. When it
hath been thus kept in fusion for about an hour, let the fire go out,
and the whole cool. Then remove the two covers. You will find adhering
to the surface of the Regulus, which will be in a mass at the bottom
of the pot, white flowers resembling snow, intermixed with beautiful,
brilliant, silver-coloured needles. Take them out, and you will find
them make about one part in sixty-two of the whole Regulus employed.
Put the covers again in their places, and proceed in the same manner
as before; when the vessels are cold you will find half as many more
flowers as you got the first time.
Proceed thus till you have converted all your Regulus into flowers.
This will require a considerable number of sublimations, which, as you
advance, will always yield you a greater portion of flowers; respect,
however, being had to the quantity of Regulus remaining in the pot.
_OBSERVATIONS._
We must here repeat what we said just before, in our observations on
the preceding process; _viz._ that Regulus of Antimony is capable of
being wholly elevated and sublimed by the action of fire; but that it
must at the same time undergo a considerable change and alteration.
These flowers of Regulus of Antimony are very different from every
other Antimonial preparation. They resemble the Pearly Matter in this,
that they cannot be reduced to a Regulus by any means whatever: but
they differ from it, 1. in that they are not fixed; for, when melted
by fire, they fly wholly away in vapours: 2. in that they are capable
of being dissolved by _aqua regis_, much in the same manner as the
Regulus; whereas the Pearly Matter is known to be indissoluble by any
Acid.
As soon as Regulus of Antimony is in fusion, it begins to sublime into
flowers; so that it is needless to apply a greater degree of heat than
is just sufficient to melt it.
A pan of some width is preferable to a crucible for this operation;
because the upper surface of the Regulus melted therein is larger,
and, the larger that surface is, the more considerable is the quantity
sublimed from it.
The two covers which are applied within and over the pot are designed
to check, as much as possible, the dissipation of the melted
Regulus; yet without absolutely excluding the free access of the
air, the concourse of which is useful in all metallic sublimations.
Notwithstanding these precautions, it is impossible to prevent the
escape of some of the Regulus, in vapours that cannot be confined.
Somewhat less than three fourths of the Regulus made use of is nearly
the yield in flowers: the rest evaporates through the interstices left
by the covers, which must not be luted for the reason just assigned.
CHAP. II.
_Of_ BISMUTH.
PROCESS I.
_To extract Bismuth from its Ore._
Break the ore of Bismuth into small pieces, and therewith fill a
crucible either of earth or iron. Set the crucible in a furnace, and
light such a fire that the bits of ore may become moderately red. Stir
the ore from time to time, and, if you perceive it crackle and fly,
keep the crucible covered. At the bottom you will find a button of
Bismuth.
_OBSERVATIONS._
The extraction of Bismuth from its ore requires nothing but simple
fusion, without the addition of any inflammable matter, because it is
naturally possessed of its metalline form. Nor does it require any
flux; because it is very fusible: which allows us to melt it, and
collect it in a mass, without the necessity of fusing likewise the
earthy and stony matters in which it is lodged. These matters remain in
their first state; and the melted Bismuth descends by its gravity to
the bottom of the crucible. No greater degree of heat must be applied,
on this occasion, than is necessary to melt the semi-metal: for, as it
is volatile, part of it would be dissipated; so that much less thereof
would be obtained, if the fire were made too strong, and so much the
less as another portion thereof would be converted into a calx. For the
same reason, the crucible must be taken out of the furnace as soon as
you perceive that all the Bismuth contained in the ore is melted, and
that the button doth not increase.
The ore of Bismuth may also be treated like the ores of Lead and Tin;
that is, it may be reduced into a fine powder, mixed with the black
flux, a little Borax, and Sea-salt; put into a close crucible, and
fused in a melting furnace. In that case you will find a button of
Regulus covered with scoria. By this method rather more Bismuth is
obtained; and it is best to make use of it when the ore is poor,
because, in such a case, none at all would be obtained by the other
process. But here care must be taken to apply at once the degree of
fire necessary to melt the mixture: for, if it remain long in the fire,
much Bismuth will be lost, on account of the great volatility of this
semi-metal, and the facility with which it turns to a calx.
Bismuth is pretty frequently found pure in its earthy and stony
matrices; and when mineralized it is usually so by Arsenic, which,
being still more volatile, flies off in vapours while the ore is
melting, provided it be but in a small quantity: if there be much
of it, and the ore be smelted by fusing it with the black flux, the
Arsenic also is reduced to a Regulus, unites more intimately with the
Bismuth, becomes a little more fixed by that union, and increases the
quantity of the semi-metallic mass found after the fusion.
Though Bismuth be not usually mineralized by Sulphur, that is not
because it is incapable of uniting therewith; for, if equal parts of
Bismuth and Sulphur be melted together, after the fusion the Bismuth
will be found increased near an eighth part, and formed into a mass
disposed in needles much like Antimony.
When we come to treat of the ore of Arsenic, we shall have occasion
to say a good deal more concerning Bismuth and its ore; because these
minerals resemble each other very much.
Mr. Geoffroy, son of the Academician, hath shewn in a Memoir read
before the Academy of Sciences, that there is a great resemblance
between Bismuth and Lead. That Memoir, which contains only the
beginning of Mr. Geoffroy's course of experiments, proves that the
author supports with dignity the glory of his name. It is there
demonstrated, by a very great number of experiments, that fire produces
the same effects on Bismuth as on Lead. This semi-metal is converted
into a calx, into litharge, and into glass, as Lead is; and these
productions have the same properties as the preparations of Lead made
with the same degree of fire. Bismuth is capable of vitrifying all the
imperfect metals, and of carrying them off through the pores of the
crucible. So that Gold and Silver may be purified and cupelled by its
means, as well as with Lead. You may on this occasion turn to what we
have said concerning Lead.
PROCESS II.
_Bismuth dissolved by Acids. Magistery of Bismuth. Sympathetic Ink._
Into a matrass put Bismuth broken into little bits: pour on it,
by little and little, twice as much _aqua fortis_. This Acid will
attack the semi-metal briskly, and dissolve it entirely, with heat,
effervescence, vapours, and puffing up. The solution will be clear and
limpid.
_OBSERVATIONS._
Of all Acids the Nitrous is that which best dissolves Bismuth. It is
not necessary, on this occasion, to place the phial, in which the
dissolution is performed, on a sand-heat, as in most other metallic
dissolutions: on the contrary, care must be taken not to pour on all
the _aqua fortis_ at once; because it operates with so much activity
that the mixture will heave up and run over the vessel.
The bare addition of water is sufficient to precipitate the solution
of Bismuth. If this solution be mixed with a very large proportion
of water, the liquor grows turbid, appears milky, and deposites a
precipitate of a very beautiful white. This is that white which the
ladies use at their toilets.
Water produces this precipitation by weakening the Acid; which probably
is incapable of keeping the Bismuth dissolved, unless it have a certain
degree of strength.
If you would have a Magistery of Bismuth beautifully white, you must
perform the dissolution with an _aqua fortis_ that is not tainted with
any mixture of the Vitriolic Acid; for this gives the precipitate a
dirty white colour, inclining to grey. Several authors advise the use
of a solution of Sea-salt, instead of pure water, for precipitating
the Bismuth, imagining that this Salt will effect a precipitation here
as it does in the cases of Silver and Lead. But Mr. Pott, a German
Chymist, who hath published a long dissertation on Bismuth, pretends,
on the contrary, that neither Sea-salt, nor its Acid, is capable of
precipitating this semi-metal; and that when a precipitation takes
place on mixing them with our solution, it is brought about only by
means of the water in which those substances are diffused.
Bismuth may also be precipitated by the means of Fixed or Volatile
Alkalis; but the precipitate is not of so fine a white as when procured
by the means of pure water only.
If a greater quantity of _aqua fortis_, than that prescribed in the
process, be made use of to dissolve the Bismuth, a great deal more
water will also be required to precipitate the Magistery; because there
will be much more Acid to weaken. This white ought to be well washed,
in order to free it from any remainder of acidity; and it should be
kept in a bottle well stopped; because the access of the air makes it
turn brown, and if any of the Acid be left it will turn it yellow.
A solution of Bismuth prepared with the proper quantity of _aqua
fortis_, that is, with two parts of the Acid to one of the semi-metal,
concretes into little crystals almost as soon as made.
_Aqua fortis_ not only acts on Bismuth when separated from its ore,
and reduced to a Regulus, but attacks it even in its ore, and likewise
dissolves at the same time some portion of the ore itself. With
this solution of the ore of Bismuth Mr. Hellot makes a very curious
Sympathetic Ink, differing from all that were known before.
Mr. Hellot prepares the liquor in the following manner: "He bruises
the ore of Bismuth to a coarse powder. On two ounces of this powder
he pours a mixture of five ounces of common water with five ounces of
_aqua fortis_. He does not heat the vessel till the first ebullitions
are over. He then sets it in a gentle sand-heat, and lets it digest
there till he sees no more air bubbles rise. When none appear in this
heat, he increases it so as to make the solvent boil slightly for a
full quarter of an hour. It takes up a tincture nearly of the colour
of brown beer. The ore that gives the _aqua fortis_ this colour is
the best. He then lets the solution cool, laying the matrass on its
side, that he may decant the liquor more conveniently when all is
precipitated that is not taken up by the solvent.