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A reading of Lully's Alchemical Experiments

There is an interesting 17th century alchemical compendium:-
Paracelsus Of The Chymical Transmutation, Genealogy and Generation of Metals & Minerals. Also, Of the Urim and Thummim of the Jews. With An Appendix, of the Vertues and Use of an excellent Water made by Dr. Trigge. The second Part of the Mumial Treatise. Whereunto is added, Philosophical and Chymical Experiments of that famous Philosopher Raymund Lully; Containing, The right and due Composition of both Elixirs. The admirable and perfect way of making the great Stone of the Philosophers, as it was truely taught in Paris, and sometimes practised in England, by the said Raymund Lully, in the time of King Edw. 3. Translated into English by R. Turner
London, printed for Richard Moon at the seven Stars, and Hen: Fletcher at the three gilt Cups in Paul's Church-yard. 1657.

Contained in this is a work of practical experiments by the supposed Raymond Lully. These are likely to have been written in the seventeeth century based on some earlier publications of 'Lully' experiments in Latin and German.

Philosophical and Chymical Experiments Of the Famous Philosopher Raymund Lully. Wherein is contained, The right and true Composition Of Both Elixirs and Universal Medicine: The admirable and perfect way of making the great Stone of the Philosophers, as it was truely taught in Paris, and sometimes practised in England by Raymund Lully in the time of K. Edward the third. Now for the Benefit of all Lovers of Art and Knowledge, carefully translated into English, out of High-German and Latine, by W.W. Student in the Celestial Sciences, and Robert Turner.

The text is one of those works of practical alchemy in which the experiments are simply described. Unlike other texts of practical alchemy which obviously on purpose code or obscure the meaning of the terms involved, this would appear to be a straightforward account of a series of experiments. We will just look at the first 'experiment' which is in chapters 1 and 2 and give a reading of the text into modern chemical terms.

Chapter I.
Teacheth, how to prepare the Salt
for the white and red Elixir.
Take, in the Name of God, great Bay-Salt as it is made out of the Sea; take a good quantity and stamp very small into a stone-Morter : then take Cucurbites of Glass, and pour your Salt therein: then take fair Well-water, and let your Salt resolve into cleer water; being all dissolved, then distil it by Filter; that is to say, hang a jag Felt or Woolen-cloath, in the Cucurbite; and let the other end hang in another Glass beside it, set as it were under it, that the Water may drop into it, that the Felt or Cloath will draw out, and that shall be cleer as Silver: and when that all the water is dopped over, look to it if that it be very cleer; if it be not, filter it again into another Glass, till it be cleer or Christalline: and when it is so, put it into a Glasen Pan, set it upon a Sand-Oven, and let the Water vapour away, till that it do come above like unto white-Salt: then take stone-piss-Pots, or Pots made of Cullen-Earth, such as the drinking Pots be made of, and put the Water and the Salt that remains, therein, and set upon the said Oven, and let it vapour away; and while that it doth dry, stir it with a stick, till that it be very dry, otherwayes, it will come into a lump or mass: and this being well dried, beat it in a stone- Morter very fine, as you did before, and then put it into a melting Cruce, and set them into a glowing Oven, or Say-Oven, which is an Oven that the Gold- smiths do enamel their Rings in: the Oven being very hot, take the Cruses that be filled with Salt, and set them into the Oven, and let them stand until they be glowing hot; and see that they be no hotter behinde then before: if they be, then turn them round with a pair of Gold-smiths Tongs: put but one Pot in the Oven at a time, that you may do them the better; and when that Pot is red glowing hot, take it out, and put it in another to be calcined.

And then, when cold, put it again into your Morter, and break it as small as you can, the third time, and then set it in the Fire of the Oven to glow as aforesaid, Two or three times glowing, and breaking of it every time in a stone-Morter until seven times, and then put it into Well-water to dissolve, till it be all dissolved into cleer water.

Then distil it by Filter, until it be as cleer as Christal, then set it again upon your Oven to dry, and the Water to vapour until that it be Salt, and stir it with a stick as beforesaid.

And when that it is dry, set it to calcine again, as beforesaid, in the Sand- Oven; and when that all the Pots that have the Salt, be all glowing hot, then take them out, and beat them to Powder, as before; and again dissolve into Water.

Then distil it again by Filter, as before: this shalt thou do so many times, to say, dissolve into Water, and then distil by Filter, and then congeal it into dry Salt, glowing it by Fire: this do without resting until it come to be fat, and that it will melt upon a hot glowing Plate of Luna: and if it will not melt like Wax, you must dissolve, distil, congeal, until that it will come to that point or perfection: and you must be careful, lest that it should melt in the Calcination; for then all your labour is lost. Keep this for a great secret: and such a preparation doth appertain to the Salt, that which is the Riches of this world.

For otherwise thou shalt never come to the perfect end of any Elixir, without such Salt prepared, as aforesaid, to say, to the white Elixir, nor yet to the red.

Therefore, my beloved Son, he that doth know the Secrets of this Salt, (to say) his Solution, his Congealation, Distillation and Calcination, and can well understand, knoweth the whole Secrets of Natural Philosophy, and wise men also; that is to say, how and in what manner he ought to dissolve, distil, congeal, and calcine. Therefore let not the labour in preparing of this Salt be grievous unto thee; for without great cost you may learn herein, to distil by Filter, dissolve, congeal, and calcine; and to form all the works that be needful unto thee in this Science.

So that you come to the principal work, you shall not be to seek or to learn: Therefore be patient, and leave not off to work, until thou hast brought thy Salt to that pass as I have taught thee before, until it melt upon a hot glowing Plate of Silver, as Wax in the fire: for without this Salt thy labor is in vain; for it is the Key of this Science.

Let us look at what the author is asking us to start with - Bay salt, that is salt created in salt pans in sea bays by evapouration. This is a natural, crude, though relatively pure form of salt.

Our author asks us to wash it and dissolve it in well water, that is pure drinking water. Then one is asked to filter it over into another vessel using a capillary filter - not the filter paper of modern chemistry, but a ribbon of cloth wetted and placed with one end in the vessel of impure substance and the other in a receiving vessel. The solution 'distils' over leaving the impurities in the cloth.

We are then asked to place this clear solution into a glass pan and heat it on a sand bath, so as to evapourate off the water. This is powdered and placed into a melting crucible and placed in an assay oven, that is one that can generate a considerable temperature - he uses the term 'glowing hot'.

The matter is taken out when cold and pounded to a powder in a mortar, and then returnd to the assay furnace, this being repeated seven times.

The resulting substance is dissolved in well water and 'distilled' with the capillary filter again. Then back to the sand bath and repeat the process.

The author then suggests that we test the resulting salt by placing it on a glowing plate of silver. If it melts like wax then you have the right result.

Now sodium chloride melts at about 850 degrees centigrade, but usually it tends to spit and boil a bit, rather than melt like wax, however, this decrepitation is due to water trapped in the crystals of salt. By heating the powdered salt to a high temperature seven times in the assay furnace, this trapped water will have been removed so the salt when heated will melt without spitting, i.e. flow like wax.
At the end of these processes one will have pure sodium chloride, mixed with small amount of Potassium Chloride and some Magnesium salts and other substances found in trace amounts in sea water.

Chapter II.
Teacheth with this prepared salt
to make the Elixir to the white work.
Take of Salt-Peter two parts, and one part of Allome, and distil thereof a strong Water.

Then take of your prepared Salt so much as you will set to work, and take as much fine Capel Luna as you have of your Salt.

Beat your Luna into thin Plates, and dissolve into the strong Water a part, in a Glass by itself.

Likewise your Salt you must dissolve in the said strong Water by it self.

And when your Luna and Salt is dissolved in both Glasses, put the two cleer Waters together, and note that you put no more Water to the dissolution of these two matters, then will dissolve them, and you shall see your Luna fall to the bottom of the Glass, white, like Milk: take the Glass properly, and shake it in your hand, and let it stand, and you shall see your Luna as a green Water to rise; above the which you shall pour properly off into another Viol of Glass: then pour upon it more strong Water, that hath not occupied, and do as aforesaid; putting the green Water off in the first green Water, shaking it, as aforesaid.

This do until all your Luna be dissolved into green Water, that no Feces remains; otherwise, your work will not be perfected: and when you have all into cleer Water without Feces, put the same into a Cucurbite of Glass with a Helm and a Recipient, and Lute it strongly: and when your Lutement is dry, then set your Cucurbite in Balneo, and make fast to the bottom of your Glass a round Certel of Lead, like a Fol; and as your Lutement doth dry, so increase your fire a little to distil of the flame, that there shall remain no more strength in it then common water: and to know this, put a clout in the mouth of the Alimbeck: and when the clout doth begin to look yellow, pull all the fire out of the Oven; for then the Spirits of the strong Water do begin to come.

Therefore look well to your work, lest your fire be too hot, that no Spirits come of your Water; otherwise you shall fail in your work. Then let your Glass and Oven stand and cool two hours long: then take off the Helm of your Cucurbite, and have a Cover of Glass that may pass just in the mouth of your Cucurbite, wherein your Medicine is in, fast luted to with Lutement, or with white Wax: then set it in your Sand-Oven, or warm Ashes, not very hot.

Then take fair Capel Luna beaten very thin into Plates and cut into small pieces, and put in a little at a time till it be dissolved; and when that is dissolved, put in more till it be dissolved also. And thus let your Glass stand in warm Ashes, and look that no Air go out of your Glass nor Cement.

This nourishing shall continue until it will dissolve no more, but lie in the Glass undissolved two or three days long: and then is your Medicine nourished like a Child in the Mothers Womb.

Then may you let your Glass wax cold, and you shall understand, without this nourishing the Medicine cannot ingender; and therefore it is needful that it be nourished, that it may get strength of Generation: and when your Glass is cold, lute your Glass well with good Lutement, that may indure against Water, the which I will learn thee in a Chapter apart, and let the Lutement dry by it self; then set the Glass in Balneo Maria, to putrefie fourty days long to hold it in such a heat, as the Sun in Summer: for great fire may destroy your Medicine. Therefore let your fire be alwayes of one heat: for in that there doth remain a great secret of the Medicine.

And within the forty dayes your Medicine shall be dissolved; and if it be not dissolved in forty dayes, let it stand longer until it be dissolved: for this is the primest of all the work: for the dissolution is done by heat and moisture, and congealed by heat and drowth.

This Point being obtained, you have the Key of the Chamber, and he is blessed of God that hath this point. For this is a token of goodness, for in every Dissolution and Congealation, you do augment your Medicine and Degree: for the first time it will do projection one ounce upon seven, and dissolve and congeal again; one ounce will project upon fourteen ounces, and the third time upon twenty eight ounces.

And so it goeth forth double in projection every Dissolution and Congealation.

But you shall understand that the Congealation that cometh of warmth, is no perfect Congealation; but it ought to congeal in the Glass or in the Ampule with heat, (to say) standing in warm Ashes: and therefore, whenas your Medicine is dissolved in your Glass, let it cool; then take it out of your Balneo, and dry your Glass.

And look well to your Lutements that they be close, without any clefts to let out the Spirits; then set it in your Sand-Oven in Ashes: then put fire in your Oven, and let your fire be no greater, then that you may hold your finger in the Ashes: and so let it stand twenty four hours to congeal; if not congealed in that time, you may let it stand longer; and when you see that it is congealed, give God thanks, and rejoyce; for it is ready to do projection in this manner.

Take to project on, Fair red Copper the best that you can get, and take from him his redness, which serveth not in the work: the which you shall do after this manner.

Beat your Venus into thin Plates, and cut it in small pieces, and anoint them with this paste or pap.

Take white Arsnick and grinde it on a Marble-stone with Oyl of Tartar, that it be thick like Pap; and with this matter anoint your (Copper) Venus pieces: then take great Bay-salt, and put some part of it into a melting - Pot bottom, and lay your (Copper) Venus pieces upon that: and then Salt upon them, and (Copper) Venus pieces upon that, Stratum super Stratum, till all your Pot is full: and uppermost in your Pot, let there be a good quantity of Salt: take a tile-stone, and make a round Covet for the Pot, and lute it well too; and when the Lutement is dry, set it in an Oven in fire of Calcination for twenty four hours long.

Then let it cool; and then break your Pot open, and cast the matter that is in your Pot in warm Water, and stir them with your Hand, until the pieces be clean, and that the Water comes fresh from them. Then dry them, and beat them in an Iron Morter, so small as you can. Then put your Venus, so beaten, into a Canvas Bag that is sowed close up, and round like a Ball. Then take fat Clay that is mixed with hair, and therewithal streak over your Bag, thinly, that it may dry; and when that it is dry, streak it over and over again, as it drieth, until your Clay be as thick as a Pot. Then, when your Clay is luted fast about your Canvas, take a small wooden Pin, and put through your Lutement into the Bag, that the small end may remain within the (Copper) Venus.

Then put the round Ball of (Copper) Venus into another melting - Pot, the wooden Pin downwards; but you must remember to put among your beaten Venus, Sandever, Verne , Saltpeter, (Ana.)

Then set this Pot in a wide Furnace to melt, and the Venus will melt and run out into the Pot, wherein it doth lie: and then the Venus shall be fair and white like Luna, and shall be profitable in this work: the which, without this work of Preparation, would not be as you should do your projection.

Take seven ounces of this prepared Venus, and put it into a melting-Pot, and flow it in the highest degree of fire that you can, in a wide Furnace: then put to it one ounce of fine Capel Luna; and when it is melten, as aforesaid, put to it one ounce of your Medicine or Elixir, and nimbly stir it with a wooden stick: but let no Iron come unto it: and when it is well corporated, then take it out, and cast it into an Ingot; so you have the best Luna in the World, to abide all Proofs and Examinations; and it is far more fine then that comes out of the Earth. When you have finished this Work, give God thanks, and remember the poor.

The second chapter requests us initially to take saltpetre (potassium nitrate) and alum (potassium aluminium sulphate) and distil these together to make a strong water. This strong water will be aqua fortis (nitric acid).

We are asked to take 'capel luna'. What can this substance be? This is probably a misreading for cupelled Luna, or silver purified by cupellation. The author obvious means the metal rather than a salt of silver, because he refers immediately to thin plates, possibly silver leaf. This finely ground silver is then dissolved in the acid to give silver nitrate.

One is asked to dissolve the salt prepared earlier separately in the nitric acid

These two solutions are then mixed together. The silver will be precipitated as silver chloride (the milky matter) and sinks to the bottom. You are to shake this, then let it stand till it is clear. The clear greenish water will be a complex mixture of sodium chloride, sodium nitrate and possibly some complex silver salts that remain in solution. Also silver may contain impurities, gold and copper being common, so there may be trace amounts of compounds of these metals too. The nitric acid will, no doubt, also contain some nitrogen osxide which give it a greenish/brown tinge. You pour off this green water into a separate flask and add more nitric acid to the residue in the first vessel, and repeat this till 'all your luna is dissolved into green water'. Silver chloride will dissolve in nitric acid, so one can suppose this means that you repeat this till the precipitated silver chloride is dissolved again by the added acid..

Next we are asked to take this green water and put this into a distillation flask fitted with a still head which should be sealed tightly. This is then placed into a water bath 'with a round certel of lead' attached. What this means is that a lead weight is tied to the base of the flask to keep it upright in the water bath.

The flask is being heated in a water bath, so the temperature cannot be higher than 100 degrees centigrade and in practise would be some few degrees lower. A test is made by placing a cloth in the mouth of the alembic. If this turns yellow one should remove it from the bath, as then the spirits of the strong acid come out. This probably means that oxides of nitrogen are being emitted from the nitric acid and staining the cloth. The experimenter does not want this to happen, so in this case you must reduce your fire. What is being done here is concentrating the silver nitrate solution, by gently vapourising off the water but without breaking down the remaining nitric acid in the solution.

Next let the vessel cool for two hours. Then remove the still head and in its place put a stopper which should be sealed tight. This is then placed on a sand bath but not too hot.

Chemically probably little is taking place here, except the danger of the nitric acid breaking down. Perhaps a little water is being evapourated off and the solution becoming even more concentrated.

The next stage he takes some more of his thin leaf silver and puts it into the flask with the green liquid so it dissolves. We realise that one of the primary components of this green liquid will be nitric acid, and he is even minded to test the output of the alembic at the previous stage to make sure the nitric acid is not being broken down. The flask he now puts in a bath of ashes, usually this means a low heat, and makes sure it is tightly sealed. This process appears to be continued till no more silver will be dissolved. This probably means there is then very little free nitric acid in the liquid.

Then the glass is left to go cold, and then tightly sealed with a lute that is impervious to water, and then it is placed in a waterbath for forty days, at a low heat, like the warmth of sunlight.

Within these forty days what he calls 'your medicine' will be dissolved. This solution in the flask will now most likely be a strong solution of silver nitrate with some other minor trace substances.

The author breaks off for a couple of paragraphs from describing the experiment to a general description of the 'Medicine'.

The next stage is to put the sealed flask onto a sand or ash bath and set a fire in the oven below, but only to create a heat which you can stand with your finger. This should in 24 hours make the substance in the flask congeal. It may even take a longer time that that. At then end one will have probably have silver nitrate in a close to solid form.

We are then to take copper plates and beat them into a thin foil, cut these into pieces and anoint them with a paste. This is made from white arsenic, a name usually applied to Arsenic trioxide which one is to grind on a marble slab with oil of tartar. Oil of tartar, as far as I know, is really just tartar in a wet viscous gel form. It can also mean Potassioum carbonate. We coat the copper foil pieces with this goo and place them at the bottom of a deep crucible together with salt, 'stratum super stratum', layer upon layer, right up to the top of the crucible, upon the top of which you should put on good quantity of salt, and cover this with a heavy tile which should be luted with some cement to seal in the crucible. When this is dry, this should be placed in an oven in a strong fire for 24 hours.

Now what is happening here? The chemistry is not entirely clear to me and it might be better if someone were to undertake to repeat the experiment. Copper is quite reactive metal and would be changed through this heating with salt. Arsenic Trioxide can be reduced by copper to arsenic at a red heat, so we must assume that this is taking place. The end result could be a real mush of arsenic and copper metal, together with chloride compounds, and some of the sodium as hydroxide. It is not easy chemistry to predict without actually undertaking the experiment.

Next we wait till the crucible cools, then we are to break it open and put the material into warm water. This will dissolve out the remaining salt and any other soluble compounds such as copper chloride. The remaining sludge and pieces of material that has not dissolved in the water is dried and ground to a powder in an iron mortar. He calls this material 'your Venus' though it is unlikely to consist purely of copper, but could contain some metallic arsenic and other unsoluble compounds. This is placed in a canvas bag which is sewn up to form a tight ball. Then you are to streak this with clay, and continue to build this clay up on the surface so it forms a tightly sealed call as thick as a pot. Then pierce this covering with a thin wooden pin right through to the mass at the centre.

He then remembers to remind us that we should have added to the ground up material some sandiver (a complex silicate scum formed on the surface of molten glass), some Varne/Verne (?) and Saltpetre.

We are to place this ball in a pot supported on its wooden spindle and place it into a furnace. The Venus or copper will melt and run out of the pot appearing white like silver, no doubt because it would contain a proportion of the silvery metal Arsenic.

We take 7 ounces of this white copper/arsenic and put it into a melting pot and add an ounce of silver, then add your previously prepared 'medicine' which is mostly silver nitrate. Stir well and then cast into an ingot. It is perhaps not too surprising that this will appear very similar to silver, as it will contain a large percentage of silver, alloyed with copper and arsenic.