Where have all the crystals gone?

Hi Nick and everybody,

I melted 5 g of silver leaf with 5 g of crystals of GW in a fire clay crucible with a fire clay lid with an iron weight put on. Temp. in electric furnace 2000°F. After one hour only a 4.6 g silvery button remained at the bottom of crucible. In the middle of the bottom of the crucible a gray/green mark with some light brown dots at the outside. It's a sign that some of the crystals have seeped through.

I see 2 possibilities:

1. try to beat the button in a mortar and rub it together with same weight of crystals again and melt.
2. melt the silvery button and do a projection with same weight of crystals encased in beewax and stir with iron rod.

What is the remedy Nick?
Or does somebody else have an idea?

Frank

I know we have talked about putting ceramic fabric under the lid that would squeeze down and create a better seal on the crucible. I suggest that for any future attempts. If you melt the silver down and do a projection with wax I would make sure to put the lid and weight on after rather than stirring because we know these crystals turn to fumes and have to be kept in.

Thanks again bluefloor,

your hints are always helpful. How are you getting on yourself? Yes I ordered some ceramic fabric already. Although I have the best Hessian fireclay crucibles which are dense and called "gold crucibles" that are perfect for gold melting, the alkahest crystals are obviously so penetrating that they seep through the porous wall of the crucible.

Therefore I will go for the graphite crucibles as Nick suggested although they are less resistant against the melting of e.g. sulfur than fire clay ones.

Yes I agree that at the first time the crucible should be sealed because the fumes might escape but I also think that 2000°F was too high for silver with a melting point at 1763.6 °F. >>The higher the temp. the more penetrating the substance.<< But didn't Nick say from the second time on the projection should be made encased in beeswax and stirred otherwise you won't get the stone like a glassy substance?

Frank

Frank,

Unfortunately I cannot work on GW any longer where I am at so I will be put off for at least several months. So, I wish all the others working now well.

Yes, as we have seen fired clay is very pourous so a different crucible will be nice. Also, even if it is not the first time, any time you add crystals they will be volitile and you will need a good sealed lid on. The only time you don't need a lid is when you are doing a transmutation and adding only metal and your glassy substance.

Stirring was also only mentioned for during a transmutation. This is also the only time I think that beeswax is used to encase the material, although I do not know the purpose of the beeswax. I thought in your case it might be a good idea for your second run because you did not end up with a glassy material that you could grind up to mix with your crystals, so to get them to mix good you could melt the silver first and then throw in some encased crystals so you could get a lid on before they fumed away.

Bluefloor,

Quote :

Unfortunately I cannot work on GW any longer where I am at

Hey if it is only for the smell I have some tips for you if you are interested. "What Odor" is one idea.

Quote :

I do not know the purpose of the beeswax

The purpose is to bring in the material encased in beeswax into the molten metal before the material goes up in smoke.

Frank

Yeah Bluefloor,
It makes sense.
I remember that more or less one year ago I post about it: may be this is one of these cases that need the use of precise terms to distinguish matters & phases (like in the art of navigation when you can't say "give me that" because there are a lot of "thats" on our boat and for this reasons there are a lot of funny terms even for the most simple things).

About GW: if we perform the via sicca, a dry path, we have these crystals that we lightly MELT WITH our determining metal (the same we want to obtain or Antimonium) producing a glassy material.
We can say that now we MULTIPLICATE the strength of this matter some times melting it with other crystals.
…Until we PROJECT it on the metal we choice to TRANSMUTE.
So there’s a mixing and melting, a multiplication and finally a projection (cum bee wax) to make the transmutation.

Eh? Let me know your mind.
So we can have a gentleman agreement about these terms…

Zosimo

Frank,

When I said "it" might be a good idea in my last post, I meant encasing your crystals in wax for your second run. I did not mean stirring. If that was not clear. I know Nick said that the only time stirring was recommended was for a transmutation. And that any time we add our crystals to MAKE the glassy material, or to MULTIPLY it, the crucible needs to be sealed. The crystals have their action by the fumes they make. But the glassy material itself made from metal, will not fume away. This is why we can purify it on a red hot plate. The impurities will fume away but our glassy material, THE STONE, will not. And this is why when we add the glassy material to a molten metal for a TRANSMUTATION we do not need a sealed crucible, but we should stir.

for Zosimo,

PROJECT- any time we throw, put, any material (usually encased in wax) on top of metal that is already melted in our crucible

MULTIPLY- when we increase the strength of our stone by one order by (in the dry path) heating for one hour in a sealed crucible the glass and equal weight of crystal

TRANSMUTATION- transforming of one metal to a different metal using our stone



- bluefloor

Bluefloor,

great explanations but forgive me I got you the first time already.

I see now that any time you use the crystals there is a danger that they might fume away. And when you do a transmutation you use the glassy stone and the inferior metal you have to stir it in order to make a transmutation.

In my case I can not encase the crystals in beeswax and project it on the molten silver because the beeswax ball would be too big for the tiny pool of molten silver.

I don't have the ceramic fabric paper yet.

I would be interested to know if a graphite crucible with a graphite lid weighted down by a 500g weight would be sufficient to prevent the fumes to escape and form the glassy material out of crystals and silver leaf?

Where did Nick say you would have to seal the crucible other than weight down the lid with an iron ring?

Frank

Frank wrote:

Where did Nick say you would have to seal the crucible other than weight down the lid with an iron ring?

Actually that is what I meant by sealed in this case. But I do think we are best to close that lid off as best we can with some ceramic fabric. Maybe you are right, with a graphite crucible and lid they might be so perfectly flat that it will be better with only a weight on top. I have also thought that because we are not totally sealing our crucibles that it might be good to add more crystals than metal, maybe even twice as much.

While I do not have any experience with cooking GW crystals with metals, I do have a lot of experience with high temperature furnaces and their use.

If you will allow me to make an observation or two, I might be able to help with this crucible discussion...

Based on various threads in the archives of this forum, and on Nick's descriptions and pictures in his latest book, and on the data on the web site of the company that made Nick's furnace, it appears to me that a reducing environment is needed inside the crucible.

Background: When heating something inside a furnace, one of the parameters that usually must be controlled is the environment inside the furnace - is it to be oxidizing, neutral, or reducing? Oxidizing environments contain oxygen - so things that can burn / oxidize often will. For example, get copper red-hot in the air and it will develop a coating of black copper oxide. Reducing environments, on the other hand, contain reducing agents (often carbon or carbon monoxide) instead of oxygen. Reducing environments will often reduce a metal oxide back to the metal. Put that black piece of copper in a reducing environment and heat it to an orange heat and then let it cool, and the oxides will be reduced to copper metal again, leaving the copper bright and shiny. Neutral environments are neither oxidizing or reducing. They are often implemented by filling the furnace with an inert gas, like argon.

This is important because many substances exhibit very different behaviors when heated, depending on the environment. Lead, for example, when heated in an oxidizing environment (the open air) will catch fire and burn at about 1800 degrees F, forming litharge. This is how cupellation works. In a reducing environment, on the other hand, lead can be heated well past its boiling point (3164 degrees F) and it will not change. The lead vapor will condense as bright, shiny beads of molten lead in the cooler parts of the furnace, where the temperature is below 3164 degrees.

Many substances, when heated in air (an oxidizing environment), will decompose, fume away, etc. These same substances, when heated in a reducing environment, will simply melt, and when they cool, will re-solidify, without experiencing any chemical changes or decomposition.

Now, let's look at Nick's furnace. He is using a graphite (carbon) crucible. Once that crucible starts getting hot, any oxygen in there is going to be converted to carbon monoxide / dioxide by consuming some of the crucible's carbon - thereby forming a reducing environment. The lid of Nick's furnace is a block of ceramic fiber. That material is quite porous. If you press your lips against it and blow, your breath will go through it. No matter how well this material mates with the top of the crucible, it will not make an air-tight seal. It will, however, prevent the easy exchange of air (via convection currents) between the inside of the crucible and the outside - and that's all that's needed. Nick has stated (here) that giving the crucible an air-tight seal is not necessary. During the roast, some oxygen from the outside will diffuse through the ceramic fiber lid, but as soon as it gets inside that crucible, it will burn away some of the graphite and become carbon monoxide/dioxide, maintaining the reducing environment.

So, Nick's furnace implicitly provides a reducing environment by using graphite crucibles and by preventing the easy exchange of air between the inside and the outside of the crucible. The graphite crucible sacrifices itself (burns away) in order to keep oxygen away from the crystals and metals in the bottom. A delicate balance would show that each time Nick uses his furnace, his graphite crucible looses weight.

If I remember right, those in the forum who used metal or ceramic crucibles did not have much luck. All of those would provide an oxidizing environment - little different from heating the materials in the open air. Note that electric furnaces that use nichrome heating elements deliberately maintain an oxidizing environment inside the furnace, because that protects the heating elements and K-type thermocouples.

Fortunately, it is easy to provide a reducing environment inside your crucible, as long as it is not too easy for convection currents to exchange the air inside the crucible with the air outside the crucible. Just put something carbonaceous inside the crucible, like pieces of wood, sawdust, white or wheat flour, grass cuttings, etc...

When I want to guarantee a reducing environment inside a non-graphite crucible, I fill any air space in the crucible with charcoal powder before I put the lid on. Then I encase the crucible in charcoal powder, inside another crucible. Using this technique, I have taken samples of steel up to 3000 degrees F and had them come out of the crucible bright and shiny - not a trace of oxides. Note that ground charcoal briquettes are not suitable for this purpose, because they contain a large amount of clay, which would contaminate whatever is inside your crucible. Do a google search on "homemade charcoal" - there are many pyrotechnic sites that give directions on how to make suitable charcoal. Or just grind up pieces of charcoal from a fire pit / camp fire.

It would not surprise me if the GW crystals were reducing agents themselves. If so, then bluefloor's suggestion of using extra GW crystals would probably help. Some of the crystals would fume away and consume the oxygen in the crucible, leaving the rest of the crystals to do their magic on the silver in a reducing environment. That's an expensive way to produce a reducing environment, though.

When I get to this stage of the GW process, I will just use a graphite crucible. Small graphite crucibles are quite easy to make...

- ramen

Ramen,

thanks very much you made my day!!!

Your post was extremely helpful.

Many months ago I was following a recipe of the Grand Master Glauber. The idea was to fix sulfur by heating it in a crucible with Glauber's salt. Actually he meant charcoal which was to be melted with Glauber's salt in order to fix the containing sulfur.

But I did not get his instructions right and thought he meant pure sulfur and melted it with Glauber's salt in a crucible. As everybody in chemistry knows you cannot heat up sulfur without it getting oxidized and escaping as fume. So I had to find a reducing environment, which I did by introducing nitrogen into the crucible covered by a lid while heating up. It worked well and the sulfur turned into a white substance. Later I tried it with a graphite crucible with lid.but without the introduction of nitrogen. Strangely it was successful too. Already then I learned that a lid on in a graphite crucible can keep the oxigen out and form a reducing environment.

Thank you for reminding me of my former experiences.

I think you are right Ramen. But I will still put some Kaowool below the graphite lid in order to seal it more tightly. For safety's sake.

Do you think that's a good idea?

Frank

Frank wrote:

Ramen,
I think you are right Ramen. But I will still put some Kaowool below the graphite lid in order to seal it more tightly. For safety's sake.

Do you think that's a good idea?

In order to maintain a reducing environment inside the graphite crucible, try to limit the convection currents which exchange the air between the inside and the outside of the crucible.

In other words, do whatever you think will make it the most "air tight".

- ramen

Thanks Ramen,

I'll get the Kaowool tomorrow and I think I'll seal just the edges of the graphite crucible with it put a graphite lid on and weight it down with a piece of iron. Since those crystal fumes are probably as penetrating as acid fumes or fumes of oxide of sulfur I am a little worried that they might attack the Kaowool and mess up the glassy material. But we'll see. With God's help we'll make it!

Frank

Thank you Ramen, domo arigatò!

Hi Bluefloor,
You wrote:
PROJECT- any time we throw, put, any material (usually encased in wax) on top of metal that is already melted in our crucible
MULTIPLY- when we increase the strength of our stone by one order by (in the dry path) heating for one hour in a sealed crucible the glass and equal weight of crystal
TRANSMUTATION- transforming of one metal to a different metal using our stone

Well, I took my time just to be sure and I found that I've to correct your explanations.
Sometimes words could enable our ideas to have an order and, may be, all of us to act properly.
I read G. Dorn paracelsian vocabular edited by Gino Testi, and Leonardo Fioravanti "Capricci Medicinali".

PROJECTION it's only concerning TRANSMUTATION.
Even the one from a "particular" method.
And MULTIPLICATION of course it's a preparation phase in wich we enpower our Philosophic Stone or materia vitrea, or pulvis rubra.
And now I'm questioning about three more problems .
I'd better to shut up next time.

Zosimo