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Ghislain
12-21-2009, 08:25 PM
To continue from where I left this post which originally read:

While trying to make Black Powder I found that it was almost impossible to buy
charcoal out of season. I could get art charcoal but that was expensive. I thought
I would try ordinary coal. The coal BP (http://genius.toucansurf.com/Black Powder.wmv) worked but was very slow.

The residue (http://genius.toucansurf.com/coal residue/residue from black powder.jpg ) looked glassy and red. As I found this interesting I ignited a larger amount
in a stainless steel cup... I retrieved the material and dissolved it in some water.

This water was now a dark bluey green (http://genius.toucansurf.com/coal residue/residue mixed with water.jpg ), alkaline and stinking of rotten eggs.

This mixture was filtered through some kitchen towel.
This was then placed in a large glass baking tray (http://genius.toucansurf.com/coal residue/filtered liquid in evaporation tray.jpg ) to evaporate.

The salt (http://genius.toucansurf.com/coal residue/salts from evaporation.jpg ) formed was alkaline and non-fusile.
However the salt that I tried to melt did change its property...
when water was added to both the salt that had not been calcined and
the calcined salt there was a colour difference seen here (http://genius.toucansurf.com/coal residue/calcined salt and non calcined.jpg )
at the top of the plate respectively left to right.

I have since acquired some charcoal and made BP with it and it leaves no red residue. Therefore
whatever the red residue is it is most likely from the coal.

Could anyone shed any more light on what this is?

Ghislain

P.S. The other ingredients in the BP was Sodium Nitrate and Sulfur.

More photo's Here (http://genius.toucansurf.com/coal residue )

I took some of the white salt and added it to a white wine. Here (http://genius.toucansurf.com/white wine.jpg )

The wine was quite acidic which was useful as the white powder was caustic.

I tasted the result...I'm not a coniseur of drink but I think it tasted something like brandy, and no longer sharp as it was before.

I have a problem now...I have run out of this white powder and the blackpowder that I created the red carbuncle from. I tried to make
some more black powder but it is burning differently and not creating the red carbuncle...its must be getting the ratio of the mixture right...
thing is I wrote it on a scrap of paper which I must have thrown away. I will keep on trying trial and error...I will get there :)

I have a flask digesting some of the green liquid, which I did not filter. I wasn't
sure what to do about gold so I burnt some leaf in with the black powder of this
particular mix...that was the last of the powder. I'll put up some pics later.
before I have always filtered the mix and poured it in an evaporation tray. the mix
usually went clear in a day...the mix I have in the sealed flask stayed green for at
least three days so I guess something must evaporate off in the open, and that must
still be in the flask.
It has settled out now but has a lot of black sediment, which is to be expected as I did not filter it.

Ghislain

P.S. white wine is the one on the right ;)

Ghislain
12-23-2009, 05:48 PM
The wine yesterday, having stood with a cardboard cover over it,
looked a little redder. Today it looks the same.

Here (http://genius.toucansurf.com/wine test.jpg ) you can see the difference between the first and second day.
First at the top, second below.
Every effort was made to get the pictures the same.

A little powder was put with a little spirit of wine, but it was very little.
There was no noticeable colour change so it is assumed that what changed
colour must have been in the wine.

Any suggestions as to why this changed colour would be welcome.

Does wine have any properties like litmus?

Ghislain

solomon levi
12-23-2009, 06:46 PM
From my experience, a sulphur tincture will be red in color.

Ghislain
12-26-2009, 11:10 AM
Thanks Sol' What would a sulfur tincture be used for?

The red residue is still stubborn, It will not form.

Before when the coal was used I put the excess ground coal in a flask, but then
continued to grind more coal from different lumps and this went on top.

With the possibility that the materials needed were only present in that one
particular lump I emptied the flask and took some powder from the bottom.

I mixed some black powder, to the best of my knowledge, the same way I had
done the first but a strange thing happened - when trying all different ways to
reproduce the black powder, and there were many attempts :(, all the results were
the same, the cup just contained some black sooty residue. This time however
the black powder produced a white residue (http://genius.toucansurf.com/coal residue/white residue.jpg ) similar in texture to the red.
A tiny sliver of the red can be seen on the left.

Could it be that something is trapped in the coal and starts to deteriorate once the
coal is broken open?

Ghislain

Ghislain
12-28-2009, 01:42 PM
The red liquid now has a scum (http://genius.toucansurf.com/coal residue/red mix float.jpg) on it. Is that an oil?
If it is how do you collect it? I tried a small feather
out of a cussion but it seemed to just move it around
and if it did collect on the feather what do you do
with it after that?

Another thing. I put some of the red liquid in another
glass and poured some more of the same white wine that
was used at the start into it. The red turned white (http://genius.toucansurf.com/coal residue/red to white.wmv ).
I checked it with some litmus (http://genius.toucansurf.com/coal residue/litmus test.jpg ) and it went from slightly
alkaline to neutral or maybe very slightly acid.

I don't think the colour change was due to dilution.

Does this point to sulphur Sol'?

Ghislain

solomon levi
12-29-2009, 07:41 PM
Hi.
Sulphur tincture is a good medicine, mostly for lungs/breathing.
But from my research it's used for lots of things - skin problems, allergies,
muscle/joint pain relief...

See MSM - it treats the same things because MSM is an ingestible form of
sulphur, but much more bulk than an alchemical tincture - you take grams
of MSM but just a couple drops of tincture.

Read the "Oil of sulphur-vive" in the Collectanea Chemica (you can find it on
the web).

Sorry, I don't have time for links, but they're in the other sulphur thread I think.



That "scum" looks just like one of the things I would find when experimenting
with the urine and minerals to obtain their oils, but it seems more like salt crystals
than oil ??? I'd get both sometimes.


"Yes" to the red turning white thing - you've precipitated the sulphur due to
change in pH.

see this at the top of page 12:

http://books.google.com/books?id=OU5343CoQrAC&printsec=frontcover&source=gbs_similarbooks_s&cad=1#v=onepage&q=&f=false

Ghislain
12-30-2009, 06:10 AM
Many thanks Sol'

Ghislain

Ghislain
01-02-2010, 01:05 AM
I am finally homing in on the correct mix for the red
residue.
It has taken an exhaustive effort and many mixes.

A major thing this has brought to light is how
easily one could miss a vital point.

I stumbled on the red carbuncle by accident
and thought I could reproduce it whenever
required. Not so. It really does have a precise
mix.

I read a post of Androgynus:

I buy lab-grade Di-Ethyl Ether from a chemical supply store. Works great for my purposes :)

I looked up Di-Ethyl Ether and one source it listed the ingredients as Ethanol and Sulphuric Acid. I think it said 5:9 ratio respectively, may have been other way
around, I can't find the original post. I thought I might try producing some.
One thing it failed to mention was how dangerous it is but the other was how difficult. A temperature of 130C - 150C is required and above that the diethyl ether
dehydrates to ethylene. You have to deliver the ethanol in drips and collect the distillate...:) I think I will buy this.

Getting to the point...IMO the things I need to know will come to me because
I want them to. If I recognise them when they do is a different matter.
This is where I appreciate being among such people as yourselves.

I am reading, but I am a slow reader and much of what I read may be red herrings \o/
how does one know?

Ghislain

Ghislain
01-13-2010, 03:41 PM
I created the red residue, unfortunately by accident
once again...however it made me realise how strong the red stuff is.
Placing it in water immediately turns the water green whereas if I
try it with the residue not red it only taints the water green. Plus the
effect on ones skin is most apparent...it is much more caustic.

Back to the drawing board :(

Ghislain

solomon levi
01-13-2010, 08:24 PM
Hi Ghislain.
See here on page 110.

http://books.google.com/books?id=nntKEQVzHP0C&pg=PA22&lpg=PA22&dq=glauber+red+carbuncle&source=bl&ots=mOTSgtF0YZ&sig=SR5JYsSAI797SdUXQL5-k-gZML4&hl=en&ei=rSpOS9eSKJDWsQPv5dXHBw&sa=X&oi=book_result&ct=result&resnum=1&ved=0CAgQ6AEwAA#v=onepage&q=glauber%20red%20carbuncle&f=false

You find the proper proportion by melting your sulphur,
or sodium sulphate, and then adding crushed charcoal dust gradually
until you see the saturation - that is, it stops reacting/flaming up.

At that saturation point, you should have the red salt.

Ghislain
01-13-2010, 08:32 PM
I have it :)

I think I can make it all the time now.

Here is the latest try (http://genius.toucansurf.com/coal residue/latest red carbuncle.jpg)...it is not as good as the first...
or is it better ;)

Ghislain

Ghislain
01-14-2010, 09:55 AM
Hi Sol’

Could you explain this sentence from the link you gave me?

“One drop thereof gilds over an imperial even as sulphur
does, if it be therein put".

I bought the book. It goes on to say:

“If any acid be poured into the white solution of the coals,
and that little by little, until the alkaline salt be neutralised,
a sediment will precipitate in the form of a white powder,
which, separated from the salt, and washed and dried, burns
away, and answers exactly to the mineral sulphur”.

I find it difficult to understand these texts. Is there a vagueness
to what is being said or is it just the language of the time that I
am not understanding?

Ghislain

Ghislain
01-14-2010, 10:51 AM
From page 111


Take the red carbuncle out of the
melting-pot, beat into fine powder,
and mix therewith half its weight of sal
ammoniac, powdered. Draw off by a
glass retort, so that the sal ammoniac
may bring over with it the said sulphur.
Wash off this red matter with ordinary
water.

Could you possibly shed some light on that
please Sol'?

Ghislain

solomon levi
01-14-2010, 06:14 PM
Hi Sol’

Could you explain this sentence from the link you gave me?

“One drop thereof gilds over an imperial even as sulphur
does, if it be therein put".

Gilding is like an electroplating - it gives a silver Imperial (a coin from those days)
a gold color/coating, but sulphur does this - it's not a transmutation - just a coloring.

I bought the book. It goes on to say:

“If any acid be poured into the white solution of the coals,
and that little by little, until the alkaline salt be neutralised,
a sediment will precipitate in the form of a white powder,
which, separated from the salt, and washed and dried, burns
away, and answers exactly to the mineral sulphur”.


This is what you did before when you precipitated some sulphur out of
solution - it IS sulphur. I guess he wasn't sure or didn't understand why.

I find it difficult to understand these texts. Is there a vagueness
to what is being said or is it just the language of the time that I
am not understanding?

Ghislain

I think you're not getting the language. He's being straight as far as i can tell.
:)

solomon levi
01-14-2010, 06:23 PM
From page 111


Take the red carbuncle out of the
melting-pot, beat into fine powder,
and mix therewith half its weight of sal
ammoniac, powdered. Draw off by a
glass retort, so that the sal ammoniac
may bring over with it the said sulphur.
Wash off this red matter with ordinary
water.

Could you possibly shed some light on that
please Sol'?

Ghislain

He says to sublimate the powder by adding half its weight of sal ammoniac.
Most times adding sal ammoniac, when in dry matters, is for sublimation,
as that particular salt is very volatile and carries the essence of whatever it
is mixed with over with it.
I'm sure one can do this in a stainless steel pot with a lid instead of glassware.

"Draw off by a glass retort" is just saying to sublimate them over a heat source.
Someone made a post/thread showing sublimation of sal ammoniac in a pot.
I'm not sure where - try to search for it if you're not familiar with this technique.

Feel free to ask any more questions/interpretations. I don't mind. :)

Ghislain
01-14-2010, 10:20 PM
Sol'

Thank you for your time. Although I do have futher questions:o

In sublimation you take a solid staight to a gas...is this correct?

If I am correct was the creation of sal ammoniac the one where
the result was deposited on the lid of the pot?

Found it Here (http://forum.alchemyforums.com/showthread.php?t=748&highlight=ammoniac)

What do they mean by 'draw off by glass retort' as it would appear
the resulting product solidifies as soon as it touches an obstacle
with a lower temperature than the gas?

I see blocked pipes :eek:

Ghislain

Edit: or is that what I should do...condense it on the lid of a pan?

I have a product from an experiment of mine that I mentioned
it is waxy and acidic and when heated lets of an acrid vapour
its soluable in water...could this be sal ammoniac?

Ghislain
01-16-2010, 01:06 AM
Hi Sol’

I found MSM...is it Methylsulfonylmethane? I had not
heard of it before.

Continuation of black powder residue:

While making all these failed attempts to make the red carbuncle
all the residues were put into a jar with some water. Also one experiment
where spirit of wine was mixed with the residue and digested was
thrown in for good measure...the experiment where you digest the
carbuncle with spirit of wine was attempted but not being sure of how much of each
and as the SoW supply was low I was a bit sparing for want of a better word.
All that resulted was a slight yellow tinge with a lot of sooty sediment...
so I threw it in the jar... can’t stand to waste anything...is probably my downfall.

The jar was left to settle and the liquid poured out carefully so as not to disturb
the sediment. This was filtered to a pale green liquid (http://genius.toucansurf.com/coal residue/settlement of waste.jpg) and then distilled (http://genius.toucansurf.com/coal residue/waste first round.jpg), taking off about one fifth.

The left over liquid was placed back into the original jar with all the black
sediment, while still hot. This seemed to extract a great deal more of
the green. It was left to settle for an hour and then the process above
was repeated.

After distilling off about another fifth the liquid (http://genius.toucansurf.com/coal residue/second mix distilation.wmv ) started to bubble like soap.
The left over liquid was placed into a dehydration tray. At this time it
was a clear dark green liquid, but soon a black sooty sediment (http://genius.toucansurf.com/coal residue/dehydration tray.wmv ) precipitated
out.

Not sure where to go from here. Is getting late, will continue this tomorrow.

Ghislain

solomon levi
01-19-2010, 07:03 PM
Sol'

Thank you for your time. Although I do have futher questions:o

In sublimation you take a solid staight to a gas...is this correct?

If I am correct was the creation of sal ammoniac the one where
the result was deposited on the lid of the pot?

Found it Here (http://forum.alchemyforums.com/showthread.php?t=748&highlight=ammoniac)


Yes. All this is correct.


What do they mean by 'draw off by glass retort' as it would appear
the resulting product solidifies as soon as it touches an obstacle
with a lower temperature than the gas?

I see blocked pipes :eek:


Yes. that would be a concern, depending on what type of glass you use.
Like there's the salt volatilisation pic by Steve Kalec that was recently
posted, and you see those salts gathering in the arm of the retort.

I'd go with the pot.

Ghislain

Edit: or is that what I should do...condense it on the lid of a pan?

I have a product from an experiment of mine that I mentioned
it is waxy and acidic and when heated lets of an acrid vapour
its soluable in water...could this be sal ammoniac?


I'm not sure. All those are also properties of sulphur products.
:)

Yeah, that's the MSM.
It's a good product. I'd just rather make it myself, or something like it,
than pay for it.
The oil of sulphur-vive (see thread) gave very similar healing properties in my experience,
and is very simple to make.

I'll contemplate your experiment some more.

Ghislain
01-20-2010, 12:13 AM
I dried the green liquid to salt...as the black soot precipitated
the liquid turned red. I mixed the salt with the waxy substance
I suspected of being sal ammoniac...it instantly started to react
I could hear a fiz and was aware of acrid vapours.

To sublimate this my planned apparatus (http://genius.toucansurf.com/coal residue/sublimation vessel.jpg) was to put a small s/steel cup into a
s/steel pan. A lid was placed on the pan and kept cool with a wet
cloth while the bottom of the pan was heated. The small cup heated
and the mixture released copius amounts of what smelled of ammonia.
The condensing vapours could be heard dripping off the lid onto the
bottom of the pan and sizzling.

This process was continued for approximately 20 mins...as a result there
was no deposit on the lid...there were some dried up marks on the
bottom of the pan but not the deposit expected. The cup now contained
a solid lump of the mixed materials.

The lump was ground in a mortise & pestle placed back into the pot and
calcined with a blow torch under the pot...the blackened powder turned
pure white except for a thin layer on top. The torch was not applied to
this as I didn't want to apply an open flame to the mix therefore when the
mix was again ground it had some discolouration.

I placed this powder back into the liquid distilled off at the beginning.

I have no idea what I am doing :D I do know I need to read up on sublimation.

Ghislain

theFool
01-27-2014, 08:44 PM
I stumbled on the red carbuncle by accident
and thought I could reproduce it whenever
required. Not so. It really does have a precise
mix.

Ghislain, probably what you have there is sodium nitrite (NaNO2). It forms when your sodium nitrate in the "BP" is in excess. I have seen it forming in powders involving sugar and sodium nitrate. It should be white in color. Yours is red either because of coal impurity or because of sulfur used. You can test very easily its presence by pouring some drops of HCl on it, it will fizz and produce the characteristic smell of NO2 fumes.

What you have here in this pic (http://genius.toucansurf.com/coal%20residue/white%20residue.jpg) is white sodium nitrite. It would be interesting to find out why sometimes it is red and sometimes white. Mix charcoal with sodium nitrate in excess, it will form again.

My interest to this chemical has been rekindled due to my research on how to dissolve gold leaf in a different way than using AR. Some experiments are showing me that NO2 gas can interact with gold. It would be interesting to try to dissolve gold with sodium nitrite..