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Distillation

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Distillation

‘Some peculiar furnaces and compendious ways of distilling…’
Glauber, Furni novi philosophici (Amsterdam, 1651), Sig. B1r.

Distillation1
Johan Isaäc Hollandus, Opera mineralia, et vegetabilia, sive de lapide philosophico… (Arnhem, 1616), p. 25.

Distillation was one of the most important chymical processes engaged in by the early modern chymist. It was a topic about which every chymist had a view and Worth’s academic and popular textbooks provide us with a wealth of information about the processes involved. For John Freind at Oxford distillation was ‘the Ascentuated Elevation of Particles, which afterwards descend again in the form of Drops’. Both Lémery and Wilson defined the process as being of two kinds: distillation ‘per ascensum… when the fire is put under the Vessel that contains the matter which is to be heated’ and ‘per descensum.. when the fire is placed over the matter that is to be heated’.

Lémery provides us with a number of plates of various instruments involved in distillation, with corresponding explanatory notes. His first table, illustrated below, was of a ‘fixt Reverberatory Furnace with one Retort’ and the key was as follows:

a. The Ash-room.
b. The Hearth or Fire-room.
c. The Retort supported by two bars of Iron.
d. The Dome.
e. The small Chimney.
f. The Receiver.
g. The Dome separated from the Furnace.
h. i. A Fixt Reverbertaory Furnace with two Retorts without a Receiver.
k. l. The Necks of the Retorts.
m. The Dome with its Stopple.
n. The Dome taken off without its Stopple.
o. A Retort.
p. The small Chimney separated.
q. A moveable melting Furnace with its holes or Registers.
r. An Iron Tripod for supporting it.
s. The Dome which consists of two pieces.
t. The Small Chimney.
u. A Pot of Earth with a hole in the middle of its height.
x. A Stopple for that hole.
y. Three Aludels of Earth.
z. A Glass-head.

Distillation2
Nicolas Lemery, A course of chymistry… (London, 1698), Table I.

Lémery explains the process of the distillation of  Guiaicum, one of the favourite treatments for syphilis in early modern Europe, as follows:

On distillation of Guaiacum.

This operation is a separation of the liquid parts of Guaiacum, from its terrestrious matter.Take the shavings of Guaiacum, fill a large Retort with them three quarters full, place it in a Reverberatory Furnace, and joyn to it a great capacious Receiver. Begin the distillation with a fire of the first degree, to warm the Retort gently, and to distill the water, which is called Phlegm; continue it in this condition, untill there come no more drops, which is a sign that all the Phlegm is distilled. Throw away that which you find in the Receiver, and fitting it again to the neck of the Retort, lute well the junctures. You must afterwards encrease the fire by degrees, and the Spirits and Oil will come forth in white clouds; continue the fire untill there comes no more, let the vessels cool, and unlute them, pour that which is in the Receiver into a Tunnel lined with brown paper, set upon a bottle, or some other vessel, the Spirit will pass through, and leave the black, thick, and very fetid Oil, in the Tunnel; pour it into a viol, and keep it for use…

The Spirit of Guaiacum may be rectified by distilling it by an Alembeck, for to separate a little impurity that might have passed with it; it works by perspiration, and by Urine: the dose is from half a drachm to a drachm and a half. It is likewise used mixt with the waters of honey, to cleanse inveterate Ulcers.

You’l find in the Retort the coals of Guaiacum, which you may turn into ashes by putting fire to them, which they will soone take than other coals: Calcine these ashes some hours in a potters furnace, then make a Lixivium of them with water, which being filtered, evaporate it in a glass or earthen vessel in sand; there will remain the Salt of Guaiacum, which you may make white by Calcining it in a Crucible in a strong fire. This Salt is Aperitive, and Sudorifick; it may serve as all other Alkalis to draw the Tincture of Vegetables: the dose is from ten grains to half a drachm in some convenient liquor.

The earth, called Caput Mortuum, is good for nothing.

After this manner the five substances of all Vegetables may be drawn; but because the fire doth give them a loathsome Empyreumatical smell, other ways have been invented to draw the Oil of Aromaticks: I shall describe them in the sequel.

Remarks.

During the distillation of Spirits, you must not make the fire too strong, for they coming forth with a great deal of violence, would else be apt to break either the Retort or the Receiver.

Though the Guaiacum that is used be a very dry body, yet abundance of liquor is drawn from it; for if you put into the Retort four pounds of this Wood, at sixteen ounces to the pound, you’l draw nine and thirty ounces of Spirit and Phlegm, and five ounces and a half of Oil; there will remain in the Retort nineteen ounces of coals, from which you may draw half an ounce or six drachms of an Alkali salt.

The Oil of Guaiacum is acrimonious by reason of the Salts it has carried along with it; and it is the gravity of these salts that does precipitate it to the bottom of the water. The Oil of Box, and most others that are drawn this same way, do the like.

These sorts of Oil are good for the Tooth-ach, because they stop the nerve with their ramous parts, hindring thereby the air from entring. Moreover by means of the acrimonious salts which they contain they do dissipate a phlegm which uses to get within the gum, and causes the pain, but yet by reason of their fetid smell men have much ado to take them into their mouth.

That which is called Spirit of Guaiacum is nothing but a dissolution of the Essential salt of the Plant in a little phlegm.

The fixt salt is an Alkali that works much like others of that kind, nevertheless it is very probable that the fixt salts of Vegetables, let them be never so much Calcines, do always retain some particular virtue of the Plant they were drawn from.

If one would take the pains to Calcine the earth that remains, he would obtain a salt, though but very little of it.’

Lémery, Nicolas, A course of chymistry, pp 475-8.

Worth’s copy of Johann Rudolf Glauber’s Furni novi philosophici (Amsterdam, 1651) reminds us that different types of furnaces had specific methods of distillation. On the Furnaces webpage of this website may be found illustrations of a number of Glauber’s furnaces, including his second furnace, which was for combustible material. Glauber explains how this second furnace should be used:

The way or the manner to perform the destillation

‘When you intend to distill, then first make a fire in the furnace, that the distilling vessel come to be very hot. But if it be not fastned to the furnace, then set it upon a grate, and lay stones about it, and coales between, and so let it grow hot, and lay melted lead into the space between the two edges or brims, to the end, that the lid, when it is put on, may close exactly, so that no spirit can get through. This done take a little of the matter you intend to distil and cast it in and presently put on the lid, and there will be no other passage left but through the pipe, to which there must be applyed and luted a very big receiver. As soon as the species cast in come to be warm, they let go their spirit, which doth come forth into the receiver: and because there was but little of the matter cast in it hath no power to force through the lute or to break the receiver, but must settle it self. This done, cast in a little more of your matter, cover it and let it go till the spirit be settled: continue this proceeding so long, untill you have spirits enough: but take heed, that you carry in no more at once, then the receiver is able to bear, else it will break. And when your vessel is full the distillation not being ended, then take off the lidd, and with an iron ladle takeout the Caput Mortuum; and so begin again to cast in, and still but a little at a time, and continue this as long as you please.Thus in one day you may distill more in a small vessel, then otherwayes you could do in a great retort; and you need not fear the least loss of the subtile spirit, nor the breaking of the receiver by the abundance of the spirits: and you may cease or leave off your distilling and begin it again when you list: also the fire cannot be made too strong so that it might cause any hurt or damage; but by this way you can make the most subtle spirit, which is impossible to be done by any Retort. But if you will distill a subtle spirit through a Retort, as of Tartar, Hartshorn, Salarmoniac, or the like, you cannot do it without prejudice (though there were but half a pound of the matter in it) the subtlest spirits coming forth with force seek to penetrate through the lute if that be not good, but if that be good so that the spirits cannot pass through it, then they break the receiver, because it cannot possibly hold such a quantity of subtle spirits at once. For when they are coming, they come so plentifully and with such a force, that the receiver cannot containe them, and so of necessity must flye asunder, or must pass through the lutum; All which is not to be feared here, because there is but little cast in at once, which cannot yeeld such a quantity of spirits, as to force the receiver to break: And when there come forth no more spirits, and  the former is settled, then more of the matter is to be cast in, and this is to be continued so long untill you have spirits enough. Afterwards take off the receiver, and put the spirit into such a glass…wherein it may be kept safely without wasting or evaporating.

In this manner all things, Vegetable, Animal, or Mineral, can be distilled in this furnace, and much better then by means of a Retort: especially such subtile spirits (as by the other way of distilling cannot be saved, but pass through the lutum) are got by this our way; and they are much better, then those heavy oyles, which commonly are taken for spirits, but are none, being only corrosive waters. For the nature and condition of a spirit is to be volatile, penetrating and subtle, and such are not those spirits of salt, Vitriol, Allome and Nitre, which are used in Apothecary shops, they being but heavy oyles, which even in a warm place do not evaporate or exhale.’

Glauber, A Description of new Philosophical Furnaces… set forth in English, by J. F.D.M. (London, 1651), pp 52-4.

 Distillation3
Theodor Kerckring,

Commentarius in currum triumphalem antimonii Basilii Valentini (Amsterdam, 1671), p. 179.

None of the experiments described here should be attempted.

Sources

Freind, John (1710), Praelectiones chymicae, in quibus omnes fere operationes chymicae ad vera principia et ipsius naturae leges rediguntur, Oxonii habitae

(Amstelodami). The translation is from Chymical Lectures (London, 1712).

Glauber, Johann Rudolf (1651), Furni novi philosophici, sive, Descriptio artis destillatoriae novae; nec non spirituum, oleorum, florum, aliorumque medicamentorum illius beneficio … (Amsterdam). The translation used here is the 1651 English translation: A Description of new Philosophical Furnacesset forth in English, by J. F.D.M. (London, 1651).

Lémery, Nicolas (1698), A course of chymistry, containing an easie method of preparing those chymical medicins which are used in physick. With curious remarks and useful discourses upon each preparation, for the benefit of such as desire to be instructed in the knowledge of this art (London).

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