Preparing the Vinegar of Antimony
The preparation of Basil Valentine, with some adaptations, the
vinegar of antimony, was prepared from antimony sulphide. It was found that the native ore did not give a yield of vinegar superior to that from the chemically prepared sulphide. Furthermore, the vinegar's constitution was investigated, although its unwillingness to form well defined compounds impeded such study.
The vinegar of antimony is mentioned in many alchemistical texts, but it is Basil Valentine who gives what is probably the first account of its preparation
In his Triumphal Chariot of Antimony he writes:
The ore from which antimony is melted and made pure must be ground most subtly and finely. Put this ground material into a round
glass which is called a Phiole, and has a very long neck, and pour distilled rainwater over it until half the glass is filled. Place this flask, well sealed, in horse-manure in order to putrefy until the ore begins to ferment, and generates a foam which floats atop. Then it is the time to take it out, because such is the sign that the body has opened itself up.1
This first step in the preparation is the digestion. In later editions of the work, Kerckring adds that "six pounds of antimony require 14 pounds of distilled water 2. . ." In order to carry out this operation, two small volumetric flasks were taken (as they have a shape most approaching the Phiole, but when larger amounts of vinegar are being made, a Kjedahl flask would be even better) and into each flask six grams of antimony trisulphide were introduced. One sample was native stibnite, the other, chemically prepared sulphide. Fourteen mIs. of distilled water were poured over each, and then the flasks were sealed. Since putrefying dung generates a temperature of about 40oC, a hot water Path was prepared to maintain this degree. A common fish-tank heater keeps the temperature reasonably constant, and an inverted flask maintains the water level. These flasks were placed in the bath so that the water levels inside and out were equivalent.
Although Valentine gives no period of time requisite for the completion of the reaction, another text states that six weeks is sufficient.3 After six weeks had passed, no foam had appeared, only a very slight scum floated on the surface of the water. The flasks were left for another six weeks, but still no foam appeared.
Such a foam would probably be produced only with larger quantities in more capacious vessels. This foam would be composed of hydrogen sulphide which is generally produced by the long term action of warm water upon finely ground sulphides of metals with chemical characteristics similar to antimony.4
The next step is the distillation. Valentine continues with the process:
Now put this digested material into an alembic, well closed, and draw the water off. Thus it will taste a little sour ... '5
Here Kerckring notes a special caution in distilling.
... when we wish to distill it after digestion, there is a certain manipulation to be observed, upon which the success of the whole work depends. Thus, the alembic is to be set up so that its beak touches the water which is in the receiver or which has passed into the receiver through distillation. Otherwise, the spirit of antimony is dispersed, and the most part thereof is lost, in which case much more time is required for the work to be perfected.6
In accordance with this behest, the distillation train was set up with the takeoff tube's end under the level of water placed in the receiver. When the apparatus had been prepared, one of the flasks was opened, and the contents transferred to the round bottom flask. At this point only a very faint odor of hydrogen sulphide was noticed. The receiver was kept cool, and the flow of gas through it was monitored carefully to avoid too rapid an evolution of whatever volatile substances might be present. After all the liquid had distilled over, the most part of it was removed and quickly sealed in a bottle,' only enough was left in the receiver so that the end of the takeoff adapter was under the liquid's level.
The sublimation follows next, for Basil states that "... when all the water comes over, then augment the fire so that a sublimate comes forth.7 Kerckring gives a more definite procedure in his commentary.
When all the water has passed through the alembic, the fire (as the author advises) is to be increased, and continued without intermission for three days and nights.8
Thus, the electric heating mantle was turned up to the highest setting which could be maintained with safety. The temperature, as recorded by thermocouple, rapidly rose to 400oC. This temperature was maintained for the required three days. By the end of this alloted interval, the head was covered with a coating of sublimate whose color varied from yellow to vermillion to deep red.
A repetition of the operations results in fortification of the "vinegar" Basil writes:
Grind this material under the feces, and pour the water upon it again, and distill it off again, and thus it becomes sharper. This operation must be repeated so often until the water becomes as sour as ordinary sharp distilled winevinegar, and the sublimate becomes less and less.9
And Kerckring adds:
Then let it cool, and, as he teaches, let the sublimate be mixed with fresh antimony. Again go through the work for three days and nights, and thereupon repeat this thrice, and then your water will be acidic like common vinegar.10
Accordingly, the brightly colored sublimate was scraped from the head, and the glittering array of crystals of antimony sulphide which had sublimed in a ring just above the limit of the heating mantle were mixed and finely ground together. At this point two methods can be followed, for when the distillate is poured over the material, the slurry can either be allowed to stand for a while, or be distilled immediately. The latter plan is much to be preferred even though it seems logical to think that digestion would produce a greater product yield. This is not the case, however. There should be no delay in distilling the material during the repetitions. if, in fact, the vinegar is left on the material for a day or two, it will actually be weaker after distillation.
Nonetheless, if the digestion is allowed to continue for a day before distillation, the matter in the flask will resolve itself into three distinct substances during the sublimation. These are: 1) a red amorphous powder in the head, 2) the array of black crystals at the limit of the mantle, 3) a tan compound at the bottom. Analysis shows the red sublimate to be the common red allotrope ot antimony sulphide; the black crystals are, of course, antimony sulphide of the black form; and the tan powder (a substance which is not changed by high heat, and is insoluble even in aqua regia) was SB2, (OH)2, S2,
However, if the distillation is done immediately, little or no hydroxysulphide is formed. In this case, the vinegar increases in pungency, at which point I will caution investigators that inhalation of the vapors of the "vinegar" will result in violent Headaches.
The Constitution of the Vinegar
A reasonable mode of proceeding in the determination of the constitution of the vinegar would be to first ascertain whether its chemical composition is that of common products arising from sulphide reactions. There are three sulphur compounds which are routinely produced from sulphides. These are: 1) hydrogen sulphide, H2S, 2) sulphurous acid, H2SO3, and 3) sulphuric acid, H2SO4.
Hydrogen sulphide is easily produced from metallic sulphides by mixing them with acids, and can be quickly recognised by its powerful and sickening odor of rotten eggs and, in solution, by the precipitation of metallic salts as sulphides. This foul gas could be produced by the effect of water on heavy metal sulphides over a long period of time, but the vinegar of antimony neither exhibits this odor, nor provokes any blackness from lead acetate. Although some odor of this gas was faintly detected on opening the digestion flask, whatever quantity was present passed off before or during distillation, and was not at all present in the distillate. As stated previously, larger quantities of the sulphide would most likely evolve a foam or scum of minute bubbles of this gas during the "putrefaction."
Both sulphurous and sulphuric acid could arise from the decomposition of metallic sulphides. The sulphurous would be quite predominant, however, and the sulphuric acid would be generated mostly through the air-oxidation of the aqueous solution. Both acids can be detected by their precipitating solutions of salts of the alkali earths, particularly barium. An aqueous solution of barium chloride was not affected by the "vinegar."
Titrations with NaOH in order to form identifiable salts failed since the vinegar's acid refused to remain combined with the alkali. An endpoint by phenolphthalein is readily found, but on standing, the color grows more intense, and the acid (which is quite volatile) escapes into the air.
The "vinegar" also refuses to precipitate any metallic salts in aqueous solution, and has no visible effect on organic reagents.
At this point it seems inevitable to conclude that the acidity and odor of this so-called "vinegar" is due to a complex sulphur acid with a very low K2. A technique to analyse this compound is now in progress, but the manipulations involved in its concentration and isolation are complex, as they rely upon a delicate form of fractional distillation coupled with fractional condensation. I propose that this compound is a highly volatile liquid boiling at about room temperature composed of only sulphur, oxygen, and hydrogen. Further isolations should yield further data, especially concerning the mechanism of its formation, its exact formula, Ka, and metallic salts. Furthermore, nuclear magnetic resonance studies are in progress, but at this point they have not yielded any important results.
Note: All translations are those of the present author made from the first editions of the original works.
1. Valentine, Basil, Triumph-Wagen Antimonii. Johan Tholde, Leipzig, 1604, p. 223.
2. Kerckring, Theodore, Commentarius in Curru Triumphali Antimonii, p. 290.
3 Weidenfeld, Johan Segeri, Secretis Adeptorum, G. Schultzen, Hamburg, 1685.
4 Mellor, J. W. A Comprehensive Treatise on Inorganic Chemistry, Longmans & Green Co., London, 1929, p. 522.
5. Valentine, p, 223.
6. Kerckring, p. 290.
7. Valentine, p. 224.
8. Kerckring, p. 290.
9. Valentine, p. 224.
10. Kerckring, p. 292.
Inquiries by Students ... and Answers
Q. Frater Albertus, what good is it to find out about the various methods to prepare plant or mineral medications when one does not know how to use them?
A. The 'good' thereof becomes only manifest when thorough tests have proven its goodness. For example, what 'good' does all the learning from a cook book do, and even the final preparation of some meals, when there is no one to benefit from them? There is presently still no other way available besides trial and error. Methods as to how to go about to find the results may vary and may be accepted or rejected, still all have but one aim: namely, to find out what is good or not good in a given instance.
Q. After finishing all the classes at the College what is one to do with the knowledge obtained? How can one use all this enormous amount of knowledge received?
A. Everyday life gives each of us the opportunity to use what we know. What we do not know is a hindrance one way or another. The more we know the better we are equipped to understand the 'Why of the How."
The more we know the better we have, or should have, control over our actions in life.
Q. The teachings in theory and in the laboratory have proven to me the great value of spagyric preparations. Since all the attention was given on spagyrics nowhere have I received any alchemistical instructions. Can these be had only in the direct way or can one receive them also through others who know about them and will teach those who are ready for them?
A. You are correct. The teachings given by the former PRS and now Paracelsus College did stress this very plainly. The reason for it is that without the spagyric process no alhernistical endeavor will succeed. It is not very well possible to enter into Algebra, Math, Calculus, etc., without the fundamentals of the simple timetable of arithmetic.
The Alchemy you speak of may be transmitted to those who are 'ready' to receive the teachings. But who is it that determines when one is ready! That is the question. Only this much can be said based on personal experience: 'When' the pupil is ready, the Master will appear. There is no mistaking about this, except if one claims by self accreditation that such a one is ready.
Q. How can the College exist and take care of all its obligations, even help those in need while attending classes to buy their food by giving them the money, or even waive the dormitory fees for those who can't afford them. What is the secret, if any?
A. No secret. We keep going as long as we have something to give. As to distributing what we have, this can take place only for as long as there is something to distribute. A distribution rests upon contribution. If you are concerned about the "secret" know that there is none as long as you love your neighbor as thyself. Maybe the "secret" only becomes noticeable when one loves oneself so much that there is nothing left to give to one's neighbor. When everything is thus kept "secret" one does not have to distribute any of the things one is entrusted with and is steward over. It still is and will be more blessed to give and distribute than to receive. Perhaps it can also be said 'Woe unto the 'Moochers' who only ask how much is there in it for me?' and by taking it let others take if there is anything left.
Q. Frater Albertus, is it really wrong to give others of the spagyric medications which I have prepared?
A. This depends on various things. First, no one is allowed by law to dispense any medication if not legally qualified. However, if one offers a visitor a cup of tea or some homemade goodies as a beverage and food supplement in form of a gesture of good will or as a present, this is not illegal. If you were to give a friend a jar of homemade preserves with the explanation what it contains and how to use it, you are not doing anything illegal. However, if you were to sell it, you would need a license to do so as you would be vending a product. You may recall one of the sayings here at the College: 'If you are in doubt don't.'