Practical alchemy archives - High-temperature distillation

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Date: 25 Jan 97 20:07:54 EST
From: Beat Krummenacher

The alchemists often used acids and bases in their preparatory work, which
they have gained from natural sources. For the preparation of the oil of vitriol
they dryly distilled sulphates, they gained the spirit of salt from a mixture of
chlorides and sulphates or chlorides and sulphuric acid etc.

The problem in such distillations is the necessary high temperature. Today
we own good furnaces, with their help the high temperatures are easily are
reached and can be maintained steadily. Against it we have today another
urgent problem: Which vessels can be used for such distillations?

If the maximum temperature totals about 500 degrees Celsius, laboratory glass
can be used. If one must distill at higher temperatures, metallic vessels or
such from stoneware, ceramics or porcelain, suit. Relating to this I have a
question: Has anyone already have gathered experience with high-temperature
distillations from ceramic retorts? I plan such distillations, and I would be
pleased, if somebody tells about their experiences.

Kind regards

Beat Krummenacher

Date: Sun, 26 Jan 1997 16:42:33 -0500
From: Gilbert Arnold

Beat Krummenacher wrote:

>Has anyone already have gathered experience with high-temperature
>distillations from ceramic retorts? I plan such distillations, and I would
>be pleased, if somebody tells about their experiences"

I have worked with vessels made from clay, both ceramic and assay
crucible high temp clay. In your part of the world, Solazaref
(France) used to make and sell excellent examples of such. However I
am trying not to use them all; making these preparations is hard on the
equipment.

I have found it necessary to learn the art of pottery; this takes some time.
In the mean time, I am using Glaubers method; for each operation, make
an LPN type furnace out of inexpensive high temp concrete with a grate
on the bottom; place coals and light, or heat the bottom with a torch, or
use a large assay crucible, cover the whole thing with a clay helmet and
direct the distillate in such a fashion that it is properly cooled and
collected. Please note that the ancients also added "pebbles" (silica).

Blessings,

Gilbert

Date: Mon, 27 Jan 1997 11:52:27 -0500 (EST)
From: J F Ruther

Hello,

What you wrote was very intersting, but I have still one question. Can you
give me a hint what << an LPN type furnace >> is?

I am looking forward to hearing from you.

Yours sincerely

J. R.

Date: 28 Jan 97 19:05:54 EST
From: Beat Krummenacher

Dear Gilbert,

Thank you very much for your statements. Today I already make my
crucibles and shells personally. Once one governs the technology, these
commodities can be manufactured simply and cheaply. Willy nilly I will
presumably have to manufacture the corresponding retorts and flasks from ceramic materials likewise personally.

As alternative to the action following Glauber mentioned by you is worth
considering. How do you arrange things, that the aggressive vapors do not
escape from the instruments?

Kind regards
Beat

Date: Thu, 30 Jan 1997 11:01:43 -0500
From: Gilbert Arnold

Dear Beat,

You may want to obtain the book "Chemical Technology 1872"
(http://www.keynet.net/~lindsay/secrets/) by Wagner published by
Lindsay publications (http://www.keynet.net/~lindsay/). Some of
Solazaref's illustrations resemble Wagner's. I seem to recall that this
book was either translated into German or was originally written in
German. It also contains a wealth of information concerning clays, lutes,
beermaking etc... This book contains diagrams that will show you how to
manage the vapors. Sometimes this is done by a series of interlinked
and cooled recipients, sometimes by bubbling. I usually adopt the spoon
by spoon approach to these types of distillation. I usually lute in the
Ayurvedic fashion, by using cotton soaked in fireclay.

Some versions of Glauber's writings have diagrams of his equipment. I
have never seen these diagrams. Another fairly good book is the Art of
Distillation by John French.

J F Ruther asked about the LPN Furnace. Diagrams of this are
probably available from PON. It is a propane gas crucible furnace.
Lindsay also carries books about gas crucible furnaces. Remember to
check if you need oxidising or non oxidising heat.

Dry distillation should be done slowly; for example, a well conducted
distillation of tartar shoul produce no smoke at the exit tubes after the
condensers.

Blessings,

Gilbert

Lindsay also carries 'De Re Metallica' by Agricola; it is also handy to
consult modern chemical technology and engineering books.

Date: Thu, 30 Jan 1997 15:09:21 -0500
From: Gilbert Arnold

An additional note re the HTD;

The Glauber type furnaces I have made to date were temporary
jury-rigged charcoal and gas fired creations made from crucible clay,
high temperatue cement, chicken wire, steel grating and fire clay bricks.
On top of which I used professionaly made helmets, retort heads and
condensing units made from clay or pyrex. Cheap to make, UNSAFE
AFTER 1 USAGE. Before making these I visited and observed in machine
shops and foundries. I watched and participated in chimney building.
And my pottery skills are very limited at this time. So if you want pottery
tips, ask Beat or Solazaref. Recently the rented farm I was working on
became unavailable. So the HTD equipment is sitting in my home
basement lab. And in a couple of years when I have the farm where I
can work in peace, I'll think about making a video about HTD but Beat and
Russ will have to be the stars because they are nicer and more
photogenic than I am.

On a more serious note, HTD is a serious work. Recently, an individual
died in an explosion doing this type of work without following safety
rules.

Further reference materials;

Hawley's Condensed Chemical Dictionary (Van Nostram Reinhold)
Phytopharmaceutical Technology (CRC Press)

Blessings,

Gilbert