Dry Distillation of Acetate Salts

[BeautifulEvil]

Dry distillation of various acetate salts can be performed in order to obtain the Philosophical Mercury needed to extract the essence from gold or other metals. I wanted to say a few things on this issue, and then perhaps ask a few questions.

If copper acetate is distilled, it yields nearly 100% pure blue-tinted radical acetic acid. Now this blue color can be removed via distillation of the acetic acid, but some say this removes its life-force, and thus will be useless in alchemy.

I remember hearing only distillation of calcium acetate yields acetone, and the others yield acetic acid or various mixtures of acetic acid/acetone/volatile oils.

Another text mentioned lead acetate is the only acetate salt we should be concerned with in the making of our secret solvent. The lead acetate is distilled until white fumes start to evolve and/or red oil starts to drip from the distillation column. The receiving vessel should be cooled below zero in order to obtain the very volatile Philosophical Mercury. The philosophical sulfur will distill over as a red oil. The acetate should be prepared using native lead ore, it should be converted to lead acetate using the radical blue-tinted acetic acid. This will result in a very energetic and living prima materia for our process.

This Philosophical Mercury is interesting because if it's digested with gold in a closed vessel it will extract the sulfur from gold and become tinted yellow. This gold Sulfur + Philosophical Mercury can then be used to create a red stone. A white stone can be created from the Sulfur of silver if extracted with the PM. A fixed stone can be made by conjoining the Salt, Sulfur, and Mercury.

Let's please get some commentary going on this path. Any of you have experience with it? Perhaps you've tried dry distillation of other acetate salts? Did your experiment yield any interesting results? I am not risking anything by revealing any "secrets" since this path is already in the public.

[ryanl]

I've distilled zinc acetate crystals and extracted a yellow liquid with it which I believe is the mercury of zinc. It smells very much like acetone and causes quite a headache. I have read that this preparation is supposed to form red oil on the surface which can be used to dissolve gold to make it potable, but I haven't noticed that at all. I put some gold leaf into it and the liquid turned blue-green in 24 hours. I have no idea what this means yet.

[BeautifulEvil]

I've distilled zinc acetate crystals and extracted a yellow liquid with it which I believe is the mercury of zinc. It smells very much like acetone and causes quite a headache.

It was probably acetone and a mixture of a few other volatile oils. Umm, you will need to start this process over again, especially if you didn't keep your samples in the freezer.

After you distill the zinc acetate, continue until the white vapor forms (this is an indicator of being near the end of the process). Be sure to use real good cooling in your receiving vessel. A calcium chloride + ice bath will work well, and should cool to around -50c. You may end up with with red oil separating, but this may not be the case. If it doesn't separate then you will need to distill the volatile liquid/oil very carefully. You should end up with a clear liquid (mercury), and then a deep red liquid (sulfur). You may want to purify the mercury and sulfur by a series of gentle distillations to remove the impurities. Purifying the mercury is straightforward, but purifying the red oil will be different. When you purify the red oil, a clear acidic phlegm will distill over first, and you will be left with a thick blood red oil in the distilling flask. This thick red oil can be distilled at higher temperatures, and is often recommended, but it can be used without further purification.

The black dragon should be calcined, and then leeched to obtain insoluble salts. These should be pure white when fully purified. The rest of the work involves combining these three parts, and is fairly straightforward (it's the same in all kingdoms). The red stone can be made from the sulfur of gold, and the white stone from the sulfur of silver. The sulfurs can be extracted from the metal by digestion in the purified philosophical mercury. The color of the sulfur of gold is yellow, and this is what the color of the philosophical mercury should be after extracting the sulfur from gold. The color of the sulfur of silver is white, and the philosophical mercury should be clear in theory.

I'm not sure what else I should say to help you. I would try the lead acetate path before the zinc acetate path. The lead acetate path is tried and true. Some people have issues with it, but I believe it's because of their technique and perhaps the impurity of starting materials.

I put some gold leaf into it and the liquid turned blue-green in 24 hours. I have no idea what this means, the gold leaf didn't liquify either.

This is most likely a compound of gold, or something similar. I doubt it's the sulfur of gold because normally the extracted sulfur takes on the original color of the metal (yellow for gold). Also, the gold doesn't have to liquefy if the philosophical mercury takes on the tint of the metal, the remaining gold means the body was left behind because only the sulfur was extracted.

[Green Lion]

Good evening.

Does it need not perform several successive distillations with zinc acetate crystals?
Once finished the first distillation (with an appearance of white smoke), we must have a clear liquid output, a small salt deposit in the cooling and caput mortuum in the ship fuel.
It then takes the clear liquid that mixes with caput mortuum and distilled again
It resumes this protocol several times.
We can use the clear liquid obtained at the last distillation to dissolve the salt deposit light of the refrigerant.
And it is on the surface of this mixture that must appear red oil after a few days.

[BeautifulEvil]

I understand what you mean Green Lion.

Odd question: have you worked with antimony or gold acetate by chance? PM me if you don't want to talk about it privately.

[Green Lion]

No, I have not worked gold acetates or antimony acetates.

[BeautifulEvil]

The dry distillation of gold acetate will create a red hue radical vinegar. This would be the BEST kind of radical vinegar to use in our works because it contains the living energy of gold.

The dry distillation of antimony acetate is something we should all consider. The antimony acetate can be made with the red radical vinegar from gold.

[Green Lion]

In the end, what is living energy of gold?
Its sulphur principle.
So you can get an equivalent from red metals such as iron or copper.
That is why some authors, who don't have any gold, preferably working on copper or iron.

[BeautifulEvil]

Its sulphur principle.
So you can get an equivalent from red metals such as iron or copper.
That is why some authors, who don't have any gold, preferably working on copper or iron.

While that may be true, the sulfur energy signature, and the quality, varies with other metals (gold being the most noble, and highest prized). The antimony acetate created from blue radical acetic acid will react differently to dry distillation than the antimony acetate created from red radical acetic acid (as in the distillation products will vary slightly). This is also true when we distill acetate salts, the sulfur created from the dry distillation varies with the metals used to create the acetate salt.

It would probably be worthwhile to leave the red/blue tint to the antimony acetate crystals (i.e. they should not be purified so as to remove the color). This will help create a more complex and energetic sulfur.

A highly energetic stone can be made from gold acetate, most definitely, but it would be rather expensive. The end product will have it's own energy signature, and it will be different than a stone created from lead or zinc acetate. Of course, then the stone from gold acetate can be multiplied to create something absolutely out of this world. I actually think the gold acetate path has been worked before, but kept hidden from the general alchemical community. I have no doubt about this, if I can come up with the idea, then I'm sure the alchemists of old knew of it.

I guess I could always work microscale. Perhaps start with a few grams of gold acetate. This should create a very small stone weighing maybe a few hundred milligrams (if that). The good thing is the gold not used in the salt of the stone can be reused.

I also wanted to add one more thing: if we SLOWLY dry distill these acetate salts we will obtain more sulfur. The more time the acetone has to act on the acetate salt residue, the more sulfur will be extracted. So keep this in mind guys. Also keep cooling in mind, cooling is VERY important. You will not catch all the volatiles if your cooling is inadequate, and really the volatiles are the some of the more medicinally beneficial components.

[Vlad]

This red vinegar from gold acetate is interesting. How do you prepare the gold acetate?
I once added vinegar to a solution of gold dissolved in aqua regia and ether extracted (I think, not sure) - but you could just boil the nitrates off. This formed a white precipitate after a few minutes of reaction. It didn't appear at first, it took a while to manifest. It's probably some strange acetate compound and not white orme gold precipitate as it didn't look the same and I made the latter already which behaves in a different manner.
So what kind of gold acetate would one go about distilling?

[BeautifulEvil]

I once added vinegar to a solution of gold dissolved in aqua regia and ether extracted (I think, not sure) - but you could just boil the nitrates off. This formed a white precipitate after a few minutes of reaction. It didn't appear at first, it took a while to manifest. It's probably some strange acetate compound and not white orme gold precipitate as it didn't look the same and I made the latter already which behaves in a different manner.

Interesting experiment. Ether extractions of gold from aqua regia yields gold chloride in the ether extract. Umm, I'm not sure what the white precipitate could be. The first test I would make is to check whether it's water soluble or not. This will tell us a lot of information.

This red vinegar from gold acetate is interesting. How do you prepare the gold acetate?

Ah, well in theory one should start with gold oxide. This gold oxide should then be calcined further to remove water impurities, but you need to keep it below it's decomposition point. This should then be reacted with a 100% radical vinegar (from copper, or silver), and then this should yield gold acetate. This gold acetate should then be dry distilled to yield the red tinted radical acetic acid. I haven't tried this experiment myself, but theoretically it should work. It may not be as easy in practice, but I'm not sure.

I need to try the experiment myself sometime.

[BeautifulEvil]

Okay, everybody, please keep in mind I haven't been completely truthful, and I'm starting to have second thoughts. My conscience is getting to me over this, and I've intentionally left out a few parts, misguided, and also added other complexities. If you try to work the process like I described, it will not work quite right.

Pay careful attention to the zinc oxide sublimate if you're doing the zinc path. This is one of the keys to the Philosophical Mercury. Also the post by Green Lion should be read carefully. Especially the part about the multiple distillations.

Contact me privately if you want more details, or search for the highly detailed post on ehow.com made by NDC.

[BeautifulEvil]

In the acetate path research papers volume 1 forward by Jean Dubuis, he mentions something called the Acetone of the Ancients.

The acetate is prepared from sea/oyster shells. These shells are high in calcium carbonate and interestingly enough also contain trace amounts precious metals such as silver, gold, and a few other notables. These metals are more concentrated in colorful shells, and it's believed only the colorful shells would be used in this process. One should go through the process of making the acetate, and evaporating to obtain the dry calcium acetate crystals. These should then be slowly dry distilled, and after a long period of decanting the distillate a red oil with interesting and beneficial properties will separate.

I'm going to give this a try sometime, as I live near the ocean and can obtain pounds and pounds of colorful shells!

[BeautifulEvil]

Right now I've got a few pounds of zinc digesting in some store bought acetic acid (5%). I've used about a gallon so far (roughly 200ml acetic acid), and I've probably got a few more gallons to go before all the zinc dissolves. I felt it would be best to start with relatively pure diluted acetic acid to create a baseline zinc acetate, and then further graduate this base zinc acetate into a living acetate with vinegar from wine or radical vinegar from copper/silver acetate.

I'll snap a picture sometime tonight and upload it, but I should say there's not much to see at this point.

[k89]

My attempt at making blue tinted radical acetic acid:

Heated some copper acetate.The molten salt started to boil releasing white fumes (quite similar to getting acetone from zinc acetate)The fumes condensed to a light GREEN(not blue) liquid in the receiver.The liquid had a pungent smell(NOT similar to vinegar). It 'bubbles' with carbonate salts, so its definitely acetic acid(or some other acid).when i added potassium carbonate to this liquid I also got a precipitate resembling copper hydroxide.Apparently some copper salt seems to have gotten into the receiver.My guess is some volatile salt of copper ended up in the receiver. The residue left in the flask is red in color ,possibly copper oxide.

[BeautifulEvil]

Heated some copper acetate.The molten salt started to boil releasing white fumes (quite similar to getting acetone from zinc acetate)The fumes condensed to a light GREEN(not blue) liquid in the receiver.

How pure was your copper acetate? The old masters state that the purity is imperative to the operation, and often they would solve et coagula many times to obtain a very pure acetate salt (i.e. all the impurities are left behind as death earth). Did you try to hold it up to a white background? Maybe it would better help you see the blue tint. I'm not sure though, I've always heard it described as being blue.

The liquid had a pungent smell(NOT similar to vinegar). It 'bubbles' with carbonate salts, so its definitely acetic acid(or some other acid).

I believe the first route is acetic anhydride, and then when it decomposes it forms very strong acetic acid. Maybe you were smelling some of the acetic anhydride? Be careful though, because both of these irritate the respiratory system.

It 'bubbles' with carbonate salts, so its definitely acetic acid(or some other acid).when i added potassium carbonate to this liquid I also got a precipitate resembling copper hydroxide.Apparently some copper salt seems to have gotten into the receiver.My guess is some volatile salt of copper ended up in the receiver.

Yes, that's most likely the case. A few alchemists mention that some of the copper will end up in the receiver flask. To remove this copper, and it's blue/green color, you can redistill it, and then you should be left with a clear acetic acid. I would only do this if you do not have to use "live" radical vinegar, because most often the copper is part of it's life force. This is still a hot issue with modern alchemists, should we redistill the radical vinegar or not?

To create more of this acetic acid, all you will need to do is add the distillate back on to the copper ashes in the distillation flask. You digest this for a little while, and then you can distill again. You may continue this until all the copper has been used, and is suspended as very very fine particles in the receiver flask.

One more thing, maybe you can titrate this acetic acid and find it's purity level. This shouldn't be too difficult if you have a reference point and some kind of ph indicator.

[k89]

How pure was your copper acetate?

The copper acetate was made from lab grade copper sulphate by precipitating copper hydroxide(with NaOH). Then,siphoning off the liquid and dissolving the precipitate in acetic acid (also lab grade).The solution containing copper acetate was dried in the sun to obtain dark green acetate crystals .The acetate may have been contaminated by copper sulphate and/or sodium sulphate.
I should probably use natural sources for better results.

Did you try to hold it up to a white background?

Yes and it was definitely a pale green.
I forgot to mention I only obtained a small quantity of radical acetic acid (20ml or so)


http://books.google.co.in/books?id=xpp1167FTqwC&pg=PA118&lpg=PA118&dq=+blue+radical+acetic+acid+alchemy&source=web&ots=2ncmwNwwBK&sig=ilv5D-EGv2dBBDvRaEacqRDEIfs&hl=en&sa=X&oi=book_result&resnum=3&ct=result#PPA118,M1
This book also says that the vinegar obtained will have a blue-green tint.


I'm going to whip up another batch of acetate salt and do the whole thing again.

One more thing, maybe you can titrate this acetic acid and find it's purity level

Good idea.
When I added the carbonate salt to the liquid there was vigorous 'fizzing' .
(much more than the usual sodium carbonate+vinegar)
I'm pretty sure that there is a very high concentration of acetic acid in it.

[BeautifulEvil]

The copper acetate was made from lab grade copper sulphate by precipitating copper hydroxide(with NaOH). Then,siphoning off the liquid and dissolving the precipitate in acetic acid (also lab grade).The solution containing copper acetate was dried in the sun to obtain dark green acetate crystals .The acetate may have been contaminated by copper sulphate and/or sodium sulphate.
I should probably use natural sources for better results.

Using lab grade chemicals is good for preliminary work, but in the end if you're doing some kind of alchemical work, it would be best to use some sort of natural source for the best results. Of course, with natural sources, you will have to purify the crude copper acetate.

I've got some copper chloride solution sitting around, but I've yet to do anything with it. I also plan on using anhydrous sodium hydroxide or anhydrous sodium carbonate (heat sodium bicarbonate in the oven). Both of these products (copper hydroxide/carbonate) will be insoluble in water, and thus should be easy to separate. I see you used lab grade acetic acid for this, and really that's fine if you plan on experimenting in general. However when preparing this for alchemy work, it would probably be best to use some sort of acetic acid obtained from a natural source, i.e. wine vinegar.

You're right about the copper acetate crystals probably being contaminated. This may be the cause of the green tint. As you know, it would've been best to purify the copper acetate, since I'm sure there are still some impurities present.

Yes and it was definitely a pale green.
I forgot to mention I only obtained a small quantity of radical acetic acid (20ml or so)

How much copper acetate did you use? More equals better, but you also need to scale up the glassware if you plan on dry distilling more copper acetate. Can you snap a shot of this radical acetic acid? I'd love to see it.

I'm going to whip up another batch of acetate salt and do the whole thing again.

I'd like to see how it turns out with the purified copper acetate. I'm sure there may still be a slight green tint, but I suppose it will be dominated by blue.

When I added the carbonate salt to the liquid there was vigorous 'fizzing' .
(much more than the usual sodium carbonate+vinegar)
I'm pretty sure that there is a very high concentration of acetic acid in it.

Oh definitely, the acetic acid should be near 99% if you didn't let it absorb water from the air. Highly concentrated acetic acid is very hygroscopic, and if you don't cap the receiver flask, it will absorb water from the air.

You seem knowledgeable though, so I'm sure you knew this. Good luck!

Oh, one more thing, what do you plan on doing with this radical acetic acid? I'm curious, hehe.

[k89]

How much copper acetate did you use?

I cant give a specific weight because i don't have weighing apparatus.
I never really allowed all of the acetate salt to decompose.Turned off the heat after obtaining a reasonable amount of liquid.This attempt was only to check if radical acetic acid distills over.

Can you snap a shot of this radical acetic acid?

Unfortunately, I don't have a camera.I plan on getting one soon.No pics till then.

Oh definitely, the acetic acid should be near 99% if you didn't let it absorb water from the air. Highly concentrated acetic acid is very hygroscopic, and if you don't cap the receiver flask, it will absorb water from the air.

You seem knowledgeable though, so I'm sure you knew this.

Actually I had no idea
But the receiver was almost air tight with a small opening to allow vapors to escape if there is a dangerous build up of pressure inside.

Oh, one more thing, what do you plan on doing with this radical acetic acid?

I came to know about 'radical acetic acid' only after seeing your posts in this thread.
My plan is to make zinc acetate using this acetic acid and then attempt the zinc acetate path.
Making the acid itself was quite an interesting experiment.I never expected the acid to have any color at all.

[BeautifulEvil]

I came to know about 'radical acetic acid' only after seeing your posts in this thread.
My plan is to make zinc acetate using this acetic acid and then attempt the zinc acetate path.
Making the acid itself was quite an interesting experiment.I never expected the acid to have any color at all.

Yeah, that's what I would do with it also. Use the radical vinegar to create exalted zinc acetate.

If I had a few ounces of silver, I would try to create radical vinegar from silver acetate. This should prove to be interesting, and I'm wondering what color the acid would be. The same for gold acetate, of course I believe gold acetate decomposes fairly quickly in the presence of water, so you would need to keep it anhydrous, or use it immediately.

Heh, indeed the acid does have color, and it's caused by some copper that has become volatilized and goes over with the acetic acid/acetic anhydride vapors. The acetic acid from silver/gold acetate should also display colors. The color can be removed by re-distilling once or twice.

[k89]

The same for gold acetate, of course I believe gold acetate decomposes fairly quickly in the presence of water

Tried to make radical acetic acid from gold acetate a few weeks back(tried this before moving on to copper acetate) .Made the gold acetate by reacting gold hydroxide with glacial acetic acid.But while drying the solution in sunlight to get the crystals out, the inside of the beaker became coated with a layer of gold. There was also a film of gold floating on the solution.I think gold acetate is photosensitive.Had to abort this experiment because
I had prepared a fairly large amount of gold acetate and it would take days to dry up if i used a hotplate.

[BeautifulEvil]

Tried to make radical acetic acid from gold acetate a few weeks back(tried this before moving on to copper acetate) .Made the gold acetate by reacting gold hydroxide with glacial acetic acid.But while drying the solution in sunlight to get the crystals out, the inside of the beaker became coated with a layer of gold. There was also a film of gold floating on the solution.I think gold acetate is photosensitive.Had to abort this experiment because I had prepared a fairly large amount of gold acetate and it would take days to dry up if i used a hotplate.

Yeah, I believe it was either the sunlight which caused the gold acetate to decompose, or the humidity/water in the air. Perhaps it was a mixture of both. Either way, that's a pretty cool experiment, and good information to know before I try this experiment.

When you created the gold acetate from gold hydroxide+acetic acid, did you notice any decomposition due to the water being created in the reaction? What did you do with this failed solution of gold acetate and elemental gold? Oh, and did you use commercial/lab grade gold hydroxide?

I would have loved to have heard/seen the end results of this experiment. I've only heard whispers of this path, and mainly I'm the only one that's been talking about it out in the open.

Next time I would try to keep the gold acetate solution in the dark as much as possible. Also, you probably use as little glacial acetic acid as possible, use only enough to convert the gold hydroxide to gold acetate. In this way you will have very little to evaporate. Also, I believe gold acetate is only slightly soluble in water, but it's highly soluble in acetic acid. So if you have very little leftover acetic acid in the reaction vessel, then it should precipitate since it's only slightly water soluble. You may also be able to salt it out if you use a highly water soluble salt which will not react with the gold acetate.

[k89]

What did you do with this solution?

Converted it back to gold hydroxide using NaOH.

Oh, and did you use commercial/lab grade gold hydroxide?

No.
I made gold chloride from pure gold metal electrolytically. Gold electrodes in concentrated brine solution with 12 volts yields yellow gold chloride solution(much safer than aqua regia or HCL + Peroxide). The gold hydroxide was precipitated from this using NaOH.

I've only heard whispers of this path, and mainly I'm the only one that's been talking about it out in the open.

Yes, this is true.Apart from your posts on the subject I cant find any material on this path.

[BeautifulEvil]

I made gold chloride from pure gold metal electrolytically. Gold electrodes in concentrated brine solution with 12 volts yields yellow gold chloride solution(much safer than aqua regia or HCL + Peroxide). The gold hydroxide was precipitated from this using NaOH.

Yes, that's a good method to use. I also remember hearing that you can create a red gold chloride solution by electrolysis also.

I will send you a PM with this method.

[k89]

did you notice any decomposition due to the water being created in the reaction?

There was no immediate decomposition.Only after being exposed to sunlight.I just found out from wikipedia that silver acetate is also photosensitive. (wikipedia)

There was a small amount of brownish precipitate . I filtered this out thinking it to be gold metal.My bad
The elemental gold was embedded in the glass.I had to wash it off thereby losing some gold.

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