The Preparation of the

True Sulphur of Antimony

+++++++++++++++++++++++++
Written by Adam Goldsmith

Copyright 2012 VITRIOL Publishing & Adam Goldsmith. All

Rights Reserved.
May not be copied, shared, or reproduced in any manner without
expressed written consent from the author, and VITROLUM
Publishing.

Page 1 of 20

In this publication Adam Goldsmith will detail a quick & simple

method for extracting the true sulphur of antimony. Included in
this guide are a number of high quality images of the process in
practice (as a proof of concept experiment).

This publication is mainly meant for quick duplication &

experimentation purposes by our students/peers. It is not meant to
be a full comprehensive publication on this subject. We leave it to
the researcher to decide upon the use of the obtained sulphur of
antimony. There are a wide variety of uses for it.

The process in part comes from Basil Valentine. He describes a

number of methods for obtaining the sulphur of antimony, but the
following method is one of the easiest ways (we describe this
method in this publication).
THE PREPARATION OF THE TRUE SULPHUR OF ANTIMONY
Also, Sulphur of Antimony is prepared in another Manner:
Grind Antimony (Adam Goldsmith: this represents stibnite) to a fine Powder,
which boil for two hours or a little longer, in a sharp Lixivium made of the ashes
of Beechwood. When boiled, filter the Antimony clear, and pour Vinegar upon
the filtered Liquor, and then the Sulphur will settle to the bottom wholly red. Pour
off the Phlegm and gently dry the Powder. Distil this Powder with Vinegar of
Wine, extract the Tincture, and do as you did with the former Sulphur. To reduce
the same into an Oil by Distilling, is worth your while: although the Oil above

Page 2 of 20

mentioned hath greater Virtues, because its Body, by the Sal-Armoniack, in the
beginning of the Sublimation was better dissolved and opened.

We do not need to use a lixivium of Beechwood ashes, but may

use pure KOH (potassium hydroxide) instead. This process will
work with a potash solution from the vegetable kingdom, but we
use commercial grade KOH for ease. We recommend trying both!

This same process may also be found in Joseph Du Chesnes A

Treatise on Metallic Alchemy.

Crocus or Sulphur of Antimony (Hepar Antimonii)

Take equal parts of antimony (Adam Goldsmith: this means stibnite) and saltpeter,
mix them well, then gradually throw this powder into a medium red-hot crucible.
Make of it Hepar or Liver of Antimony, pulverize and boil it in water till the latter
turns red. Run it through brown paper or filter it other wise, then pour either
simple or distilled vinegar into it, and suddenly the tincture or the red sulphur will
separate and precipitate to the bottom. The thus prepared and dry sulphur can
serve as a great remedy for purifying the mass of the blood, and even as an
excellent purgative.
Mr Wolfius, physician in ordinary to His Serene Highness Prince Maurice,
Landgrave of Hessen, made an interesting experiment with it in connection with a
young girl who had galls (skin sores) on her legs, so ugly and trying that he
wondered if it was not some sort of lepra. By rubbing them with Sulphur and
Mercury, the galls disappeared but came back later. To achieve a complete
recovery, he made her take some of this crocus of antimony for one month, mixed
with a diuretic extract, only in the proportion of 6 or 7 grains to 1 dram of

Page 3 of 20

diuretic, which she took in the morning. Sometimes she had 2 or 3 bowel
movements, without any disturbance or vomiting -- due to the aforesaid mixture.
After taking this remedy for one month, she was completely cured. This
experience has made him praise all remedies made of antimony more than those
made of Mercury.

Basil Valentine also mentions another process that relates to this

one to a fair degree. In the following process described by
Valentine he outlines the preparation of the liver of antimony, and
the precipitation of the sulphur from solution via the use of wine
vinegar:
THE LIVER OF ANTIMONY

Again, another Extraction of Antimony is thus instituted. Take, in the Name of the
Lord, of Antimony and crude Tartar, of each equal parts; put these well mixed
together in Powders, into a strong Crucible, which will not suffer the Spirits to
penetrate it, and burn this Matter in the Fire, until the Tartar be wholly combust:
this work must be done in a Wind-furnace. Grind this burnt Matter to a subtle
Powder, and pour on that Common Water first made hot, and so edulcorate the
Matter by Lixiviating. And so it becomes a Liver*, so called by many of our
Ancestors, who lived long before us.

Kirkringus: The Liver is a Cause of much Discourse in Banquets, and the Liver of
Antimony will be to us no small Occasion of the like in Chymical Operations. But
in the first place consider, that instead of Crude Tartar, it is better to take Salt of
Tartar, not only for accelerating the Operation (for otherwise it must be melted so
long, as until the Tartar be changed into Salt) but chiefly, that you may have

Page 4 of 20

Glass of a far better Color. Also Basilius forgot, or for some Reason did omit, to
appoint the Glass first to be poured into a Platter made hot, and then beaten to
Powder in an hot Mortar: otherwise the Glass, by reason of the Salt of Tartar, as
soon as it takes the cold Air is changed into a certain Pulse or Pap. Besides, he
omitted to determine the Quantity of Water, in which this Powder should be
dissolved, that we may have a more fair and deep Color; in which Exaltation of
Color very much is sited. Also the Precipitation of the Liver from the Water,
which must be made with Vinegar, be involved in Silence; although this, and
the above mentioned, are necessary in this Operation.

Therefore, returning to the Matter from whence I digressed, I affirm, that there
are some times of the year, in which if Liver of Antimony be made, and
precipitated with a due Menstruum, it will be imbibed with altogether another
Color, and be endued with other Virtues than that, which is made at another time;
and that, both for Metals, and for healing the Infirmities of men, as I myself have
experienced in many grievous Diseases, and Symptoms of Diseases. I will also
add this: from the Liver of Antimony may be extracted a Redness with Spirit of
Wine, which Redness is made volatile, and passeth over the Helm, which also may
be exhibited to all without danger. Nor is there any great need of that Caution of
Basilius (even before the Redness is volatilized) that it must be given in a small
Quantity. For being given from thirty to forty, or fifty Drops, it sweats
moderately, and doth not Purge or Vomit: but it affects wonders in purging the
Blood, extirpating the Roots of a Disease, and rendering the Patient vigorous, by
insensible Expiration, and its occult Virtues. This Vendible Wine needs not the
Bush of Eloquence to commend it to the Sick; who once having experienced its
Virtues, know what it can do, and that it as much answers their Desires, as they
esteem their Money.

Page 5 of 20

Put this Liver dried into a Cucurbit, pour thereon most pure Spirit of Wine;
abstract the Spirit by distilling in B.M. so that a third part only may remain. But
before Distillation, the Spirit of Wine together with the Extraction must be filtered
through Paper. This Extraction may indeed be profitably used; but in a small
Dose, and with great Caution. What happens in this Operation is very admirable.
For the Spirit of Wine abstracted, can no more be united with the red Extraction,
whence it was distilled; but one floats above the other, as Water and Oil, which
cannot be mixed. But if the abstracted Spirit of Wine be poured upon other Liver
of Antimony, it again attracts the Color to itself; yet this, although poured upon
the former Extraction, cannot be mixed therewith. Which is a Thing so strange, as
it may be numbered among Wonders. But who can declare the Wonders of GOD?
Or who will worthily esteem the Gifts of the Creator, which he hath implanted in
his Creatures? By us scarcely perscrutable with deep Meditation.

I before made mention of the Extraction of Antimony, from its Glass* by

Vinegar, and also by Spirit of Wine: but I now say, when such an Extraction is
made by Vinegar, and the Vinegar is again abstracted by B.M. and the Powder
which remains is resolved in a moist place, into Oil or Liquor of a Yellow Color;
it effects such Wonders in Wounds, new and old, as I neither can, nor dare to
commit them all to writing.

Process in Practice:
The process is rather simple. We need the material from
which we will extract our antimonial sulphur (antimony trisulfide stibnite, we used a finely divided/pulverized version can be
obtained from http://www.primamateriashop.com), an alkali salt

Page 6 of 20

(potassium hydroxide is what we used), vinegar of wine (white

food-grade 6% table vinegar can be utilized), and distilled water.
A very brief run-down of the process is as follows: add
pulverized antimony trisulfide to a flask, pour in KOH alkali
solution, stir well with glass-rod, and let it digest for a few hours at
approximately 120-140F. Do not let boil. A tincture will be drawn
while digesting (usually the tincture is slightly golden yellow, but
will vary depending on a number of factors). Take this tincture,
filter/decant it from the sediment, and slowly pour a variable
quantity of vinegar of wine until no more vivid orange/red colored
sulphur of antimony precipitates. Let settle, decant/filter, and wash
the sulphur with distilled water to remove all traces of water
soluble salt.
Be careful handling the KOH extract/tincture. Its toxic, and
very caustic. Take note of the rather peculiar smell it possesses.
Its very earthy, and actually resembles the fragrance of garlic to a
degree. Do not get it on your hands, in your eyes, or ingest it.

Materials Needed: Powdered Antimony Trisulfide, Potassium

Hydroxide, Vinegar of Wine, Distilled Water, Beakers, Flasks,
Heating/Digesting Apparatus, Funnel, Filters, Glass Stirring Rod

Page 7 of 20

1. Prepare the alkali salt solution. We use 5g KOH per 100ml of

distilled water.
2. Measure out 2g of powdered antimony trisulfide. Add this to a
large boiling flask. We pour the previously prepared alkali salt
solution onto this powder, stir, and then let it digest for a few
hours at approximately 120-140F.
3. After digestion the KOH solution tincture is decanted/filtered
from the antimony trisulfide sediment that remains. Its best to
decant what you can, and then filter the rest. This helps to keep
filter clogging to a minimum.
4. Keep the filtered/decanted sediment, and extract with fresh
alkali solution to remove all sulphur. Pool all extractions into
one.
5. Take the KOH tincture from step #4, and transfer to a larger
beaker/flask. You will need extra volume if your vinegar is
dilute with water.
Slowly pour in distilled white table vinegar. Neutralization of
any remaining KOH is taking place. Stir well, and once any
excess KOH has been neutralized the orange/red sulphur will
drop out of solution. This smells very bad. Do it outside at a
time when the wind is blowing well. Continue adding vinegar
until all the sulphur has precipitated.

Page 8 of 20

6. Let the sulphur of antimony precipitate settle. Decant, and wash

with distilled water three times, or until the water soluble salt
has been removed completely.
7. After washing, pour into a storage container for later use. A
tincture from this can be prepared using a few more steps, but
we leave this to the reader to devise. We may calculate our yield
by drying the sulphur of antimony gently, and then weighing it.
This is up to you.

Page 9 of 20

Image Showcase of the True Sulphur of

Antimony Preparation

Fig. 1 Measured 5g of KOH alkali flakes in 200ml beaker.

Page 10 of 20

Fig. 2 100ml of distilled water was added to the previously measured 5g

KOH flakes.

Page 11 of 20

Fig. 3 Approximately 2g of raw powdered antimony trisulfide (stibnite).

This is also called kohl (looks like powdered coal doesnt it?).

Page 12 of 20

Fig. 4 2g of antimony trisulfide powder was added to a 250ml Erlenmeyer

flask.

Page 13 of 20

Fig. 5 The previously prepared 100ml KOH solution was added to the 2g
powdered antimony trisulfide in a 250ml Erlenmeyer flask.

Page 14 of 20

Fig. 6 After heating for approximately one hour the solution will look like
this (I let it settle for an hour before taking this picture).

Page 15 of 20

Fig. 7 The decanted/filtered sulphur of antimony tincture ready to be

transferred to a larger vessel.

Page 16 of 20

Fig. 8 The sulphur of antimony solution in a 500ml RB boiling flask.

Page 17 of 20

Fig. 9 Another image of the sulphur of antimony solution in a 500ml RB

boiling flask.

Page 18 of 20

Fig. 10 The orange/red sulphur of antimony after addition of

approximately 300ml of white distilled table vinegar. Please note, in this
image more sulphur is still left to be precipitated if the top layer is tinged
yellow.

Page 19 of 20

Fig. 11 Another image of the orange/red sulphur of antimony after

addition of approximately 300ml of white distilled table vinegar.

FINIS.

Page 20 of 20