Re: Dry Distillation of Acetate Salts

[BeautifulEvil]

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

Ah, then gold acetate should also be photosensitive. I wonder if copper acetate is the same way? Probably not as photosensitive as the others, if at all.

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

Hehe, yes the brownish precipitate was indeed gold acetate. How much gold did you use for this? Hopefully you didn't waste very much, it's expensive!

[k89]

How much gold did you use for this? Hopefully you didn't waste very much

Possibly half a gram of gold.Been purchasing gold in small amounts for a long time.
Recovered most of it in hydroxide form.

Didn't loose too much gold.A negligible amount got embedded in the beaker glass(gives the glass a pink hue) and had to be scrubbed off.Apparently, the gold film prevented further decomposition of gold acetate by blocking off enough light.The gold acetate wasn't too sensitive to light.It was stable indoors under artificial lighting.Only sunlight seemed to affect it.

Ah, then gold acetate should also be photosensitive. I wonder if copper acetate is the same way? Probably not as photosensitive as the others, if at all.

I don't think copper acetate is photosensitive.My first batch was dried in the sun for over 3 days.Didn't notice any decomposition

[BeautifulEvil]

The gold acetate wasn't too sensitive to light.It was stable indoors under artificial lighting.Only sunlight seemed to affect it.

Odd, possibly the UV rays? I remember hearing a few other stories like this about the sun affecting alchemical processes much more differently than artificial lighting.

I don't think copper acetate is photosensitive.My first batch was dried in the sun for over 3 days.Didn't notice any decomposition

Yeah, I figured that much. Copper salts/compounds are fairly stable, so that doesn't surprise me in the least.

[k89]

preparation of gold acetate#2

I've attempted gold acetate synthesis again.
Acetic acid was added to gold hydroxide.The result was a deep green solution along with small quantity of brown precipitate(similar to the one i mentioned earlier).This precipitate was filtered out.It was not soluble in acetic acid(I think it is gold metal after all and not acetate).
I tried salting out the acetate by adding table salt but the salt simply dissolved without causing any precipitation.Gold(III) acetate is insoluble in water.But,I have a clear dark green solution.Maybe this is gold(I) acetate?I can't find information on gold(I) acetate anywhere.
I am boiling away the water and acetic acid to get gold acetate crystals.Now there is another problem,the salt I used is crystallizing out along with the acetate.Can I distill a mixture of gold acetate + salt to get radical acetic acid?Will the sodium chloride interfere in the process?
The only way of removing the salt would be to convert the gold back to hydroxide and start the process again.This is too troublesome.

[MythMath]

I very much enjoy reading about these various
processes, keep up the good work(s)...

[BeautifulEvil]

Acetic acid was added to gold hydroxide.The result was a deep green solution along with small quantity of brown precipitate(similar to the one i mentioned earlier).This precipitate was filtered out.It was not soluble in acetic acid(I think it is gold metal after all and not acetate).

Now that's interesting, maybe the gold was impure? This may be a different metal entirely. Can you heat it up in a crucible? You will need a high temperature if it's a gold salt in order to turn it back to metal.

I tried salting out the acetate by adding table salt but the salt simply dissolved without causing any precipitation.Gold(III) acetate is insoluble in water.But,I have a clear dark green solution.Maybe this is gold(I) acetate?I can't find information on gold(I) acetate anywhere.

I wish I could be of more help on this issue, I haven't performed the process yet, but the dark green solution is interesting. I doubt it's gold (I) acetate, because it seems the common way of making gold acetate is through this process, and it should yield gold (III) acetate. I'm not sure gold (I) acetate exists either.

I am boiling away the water and acetic acid to get gold acetate crystals.Now there is another problem,the salt I used is crystallizing out along with the acetate.Can I distill a mixture of gold acetate + salt to get radical acetic acid?Will the sodium chloride interfere in the process?

Well, you may try fractional crystallization. Both of these salts will crystallize in a different manner, and in this way you can separate them. To be truthful, I probably shouldn't have mentioned the salting out method. I would've just very lightly heated this solution until near dry point. Then just let the remaining 10-50 ml of liquid evaporate.

You may also use the solubility traits of each salt to your advantage. Table salt, which is sodium chloride, is highly soluble in water, and if you add just enough water to dissolve the salt, you will leave MOST of the gold (III) acetate behind. We're talking ml by ml of pure distilled water, and then stirring. If you knew the weight of table salt used you would be able to approximate the amount of water to use (35.9 g/100 mL [25 °C]).

Also you should try to purify the gold acetate as much as possible, it should be as pure as possible. You're right though, sodium chloride WILL contaminate the distillate/acetic acid. I recommend cleaning the gold acetate as much as possible before subjecting it to distillation.

Hopefully this should help some. The old alchemists were well aware of fractional crystallization, and all these little solubility tricks.

[k89]

Second attempt at destructive distillation of copper acetate:
The copper acetate was prepared the same way as before(Precipitating hydroxide from copper sulphate and dissolving the hydroxide in acetic acid.)
This time the copper hydroxide was 'washed' three times to remove any other soluble salts.
Acetic acid(glacial) was added to this hydroxide to obtain dark blue copper acetate solution.(about 700 ml).The solution was boiled down to obtain dark green copper acetate salt.

After complete destructive distillation, I have 10 ml of a pale green liquid (color is same as last time), strong irritating odor (also same as last time).There is definitely not even a hint of
blue in it.



Beautiful Evil,How did you come to know that the distilled acid should be blue-green?
(I mean what are you sources?)
Has anyone obtained blue/blue-green acid from copper acetate?
------------------------------------------------------------------------------------------------------------------
Still working on the gold acetate and things are getting weird.Initially the liquid was dark green.After boiling off all the water and acetic acid there was a gray-blue salt(NaCl+Some salt of gold) left along with some fluffy brown salt(gold acetate).This was again dissolved in water and this time the color of the solution was blue green. Now I've precipitated out the gold as hydroxide and the hydroxide is white in color.Will try to make gold acetate again.I no longer think that acetic acid +gold hydroxide is a good idea.As you said earlier the gold acetate formed is probably decomposing into something else due to the water formed in the reaction.

[BeautifulEvil]

After complete destructive distillation, I have 10 ml of a pale green liquid (color is same as last time), strong irritating odor (also same as last time).There is definitely not even a hint of
blue in it.

Beautiful Evil,How did you come to know that the distilled acid should be blue-green?

Actually, all the sources say the liquid should be blue! However, you're getting something different, which is quite interesting. The green color is equally fascinating. If you wait until I get home from work I can find references for you.

Will try to make gold acetate again.I no longer think that acetic acid +gold hydroxide is a good idea.As you said earlier the gold acetate formed is probably decomposing into something else due to the water formed in the reaction.

Here's something you can try instead. You may still use gold hydroxide, but you will need to calcine it to gold oxide. Be sure to keep the gold hydroxide/oxide under a certain temperature, or it will decompose into gold metal. You will then need to use the radical acetic acid acid to make gold acetate. This should release very little water. It may be best to double or even triple distill the radical acetic acid to remove all trace metals and salts. This will then allow for a very pure gold acetate to be formed.

[k89]

Here is picture of the radical acid made from copper acetate.It isn't very good because it was taken with a web camera and the lighting was poor but it has captured the green tint.

[k89]

I've finished working with gold acetate(finally!!)
Destructive distillation yielded a very light yellow liquid.(only about 5 ml)
The smell is similar to the liquid distilled off copper acetate.(very strong and irritating but unlike acetic acid.).
The yellow color is barely visible. I only noticed it while comparing it with a sample of water.
For making the gold acetate, I added all my gold hydroxide to acetic acid (glacial).
This resulted in the dark green solution + precipitate that I spoke about earlier.
After boiling away the excess acetic acid ,I had a gray blue salt.Gold acetate is brown.But then again ,gold hydroxide is purple, but I've made white gold hydroxide.
The salt was then subjected to destructive distillation.(It melts and bubbles like the other acetates)The residue left is gray(gold oxide probably).

The acid I distilled became white and cloudy after sometime.I think this is because some impurity got into it later.(I was storing it in a beaker with no cover).Anyway I'm going to repeat the experiment.This time I can add acetic acid to the residue(gold oxide) to get gold acetate.

I've been thinking about the dark green solution + precipitate that I get every time.
My guess is that the precipitate is gold released when some off the gold acetate decomposes due the water formed. The remaining gold acetate dissolves in the acetic acid to give the green solution.This is just my guess and is not based on scientific data.

I will post some pictures later.

[k89]

Green solution and precipitate formed on adding acetic acid to gold hydroxide



Yellow liquid distilled out of it.This is the second time I've distilled gold acetate and this time the color is more visible than the first time.



Residue left in the flask.





I've found some material that says that copper acetate gives green tinted acid.

When acetate of copper is reduced to powder and distilled at first there comes over a liquor nearly tasteless and colorless and afterwards a highly concentrated acid When the heat is continued until the bottom of the retort is red hot no more acid comes over and there remains a powder of the color of copper The acid product which should be collected in a receiver by itself is tinged green by a little copper which comes over with it; but by distilling again in a gentle heat, it is obtained transparent and colorless like water. This acid is very pungent and concentrated and it is the radical vinegar,or the vinegar of Venus of the alchemists.

source: The London encyclopedia

In the "Acetate Path resource papers Volume 1" it is said that the distilled acid has a color because it extracts the alchemical sulfur from the metal. Since the color of sulfur of gold corresponds to yellow, does it mean that the acid distilled from gold acetate should be yellow tinged?

[BeautifulEvil]

Ah, awesome developments with your work k89. I've been out of town for the past 5 days and haven't had access to the internet.

Here is picture of the radical acid made from copper acetate.It isn't very good because it was taken with a web camera and the lighting was poor but it has captured the green tint.

Ah, that's pretty cool. There is a slight green tint! I don't see any blue to it at all.

I've finished working with gold acetate(finally!!)
Destructive distillation yielded a very light yellow liquid.(only about 5 ml)

YELLOW!!! How very surprising! This is actually pretty interesting. When I thought about all this, I assumed it would look red, but alas, it does take on the color of the metal.

The salt was then subjected to destructive distillation.(It melts and bubbles like the other acetates)The residue left is gray(gold oxide probably).

I figure that's the case, probably a mix of gold oxide and gold. If it is an oxide, then this suits us well, because we can now cohobate this residue with the distillate. This will convert the gold oxide back to acetate, and then you can redistill this a few times. I wonder what will happen? Will it volatilize the gold? I wonder if the distillate will begin to take on the color of yellow more and more, maybe red even!

The acid I distilled became white and cloudy after sometime.I think this is because some impurity got into it later.(I was storing it in a beaker with no cover).Anyway I'm going to repeat the experiment.This time I can add acetic acid to the residue(gold oxide) to get gold acetate.

Cloudy you say? Another interesting development. Did you try to dissolve elemental gold in this solution? Please give it a try if you will. It would be quite surprising if you could get it to dissolve. Perhaps digest this solution with 100 to 200 mg of gold leaf/powder for a while. Maybe it will result in a red oil of gold swimming on top.

Yellow liquid distilled out of it.This is the second time I've distilled gold acetate and this time the color is more visible than the first time.

Yes, this image is MUCH better. The yellow tint is definitely visible.

In the "Acetate Path resource papers Volume 1" it is said that the distilled acid has a color because it extracts the alchemical sulfur from the metal. Since the color of sulfur of gold corresponds to yellow, does it mean that the acid distilled from gold acetate should be yellow tinged?

Yeah, I read the same documents. I guess that's the case, and it should be yellow tinged. I wonder how much we can tinge this though. Will the yellow turn orange or even red in high concentrations (i.e. if we cohobate many times)?

You're doing some very good research in my opinion. Thank you VERY much for sharing your work with the forum. I am very pleased with the results, very pleased indeed.

[k89]

Cloudy you say?

When the first batch turned cloudy I assumed it was contaminated by something.When I added a few drops of water to the second batch it turned cloudy.I think it is the water that causes this.I never tried this with the green radical acetic acid though.

Did you try to dissolve elemental gold in this solution? Please give it a try if you will. It would be quite surprising if you could get it to dissolve. Perhaps digest this solution with 100 to 200 mg of gold leaf/powder for a while. Maybe it will result in a red oil of gold swimming on top.

I wonder how much we can tinge this though. Will the yellow turn orange or even red in high concentrations

Will try this when I get time.I have a small piece of gold metal that I can use for this.I also have the gold + gold oxide residue that can be converted to acetate using the distilled acid itself.

You're doing some very good research in my opinion. Thank you VERY much for sharing your work with the forum. I am very pleased with the results, very pleased indeed.

Hehe , thank you for the encouraging words.

[BeautifulEvil]

I'm really interested to see if you can get a red oil from gold or copper via distillation of the acetates. Currently, I'm reading a process from "Secrets of the Adepts" about the dry distillation of copper acetate or noble vitriol. This is made from common copper, which is made according to our art into verdegrese. This verdegrese is then added to distilled vinegar (philosophical, vinegar mixed with the spirit of philosophical wine), filter, crystallize, and the purify multiple times with distilled water. This yields a noble vitriol, from which we can make the red oil of copper (silver, and gold in theory?). Anyway, It says the green spirit (which is what you obtained from copper acetate) will come over as a white vapor. If the fire/heat is continued and graduated after this spirit distills, then a few drops of red oil should come over at last.

These are then separated by distillation again through gentle heat, and the oil will be left in the distillation flask. The oil of venus is then used to dissolve iron fillings (rain water is added until all the iron dissolves). Then take this and draw off the phlegm via distillation. Take this and let it crystallize into a very pure vitriol. Thus mars and venus are joined together, calcine this very gently into a red powder, stir often using an iron wire.

Take this red powder of venus and mars and distill as before. A white spirit will distill first, the philosophers mercury, and then a red sulphur will distill, the philosophers sulphur. This is supposedly the oil of the green and red lion. This oil will be used to nourish the King, their Father. Take this philosophers sulfur and draw off the phelgm via distillation.

Now take the caput mortuum, the red crimson residue in the distillation flask, and grind it to a fine powder. Take philosophical vinegar, pour it on the red powder, and digest for three days in a gentle heat to extract the salt. Now it's not clear whether we should filter this, or evaporate as is, but I suspect it should be filtered to remove insolubles and impurities. Either way, take the salt and pour on to it the oil of venus and mars (philosophers sulphur). This should dissolve all the salt. Now you will need to take this and distill as before. This will then carry over its own spirit of salt with the oil.

In the end, after you complete the entire work, you should have an incombustible oil of mercury, sulphur, and salt. This should be able to transmutate metals. Also, you can use the oil of mars & venus (philosophers oil of mercury), the oil of gold, and the salt of gold to make a different version of this stone. Actually, there are many different things you can do with this, and really the entire realm is open.

The key to all this is the philosophical vinegar and the philosophers oil of mercury!

EDIT: Green Lion also made a very detailed thread about a form of this process: https://alchemy-forums.forumotion.com/practical-alchemy-f4/metallic-magister-of-acetates-path-t268.htm

[k89]

This is the way I understand it.First, heat the acetate salt to distill off the radical acid.After all the acid is distilled out,increase the heat till a red oil starts to distill over.
So, I decided to try it out on gold acetate.The acetate was made by adding acetic acid to the residue obtained from my earlier experiment.
First, I heated the acetate on a hotplate at maximum temperature(300°C) I got the yellow acid again.The process was slow.So , to speed things up I switched to a gas burner.I replaced the receiver. This once again yielded a yellow liquid BUT, this smells like the liquid obtained by dry distillation of zinc acetate.
There is a clear difference in the smell of the two liquids that I've got.This suggests that at higher temperatures gold acetate yields acetone and not acetic acid.
After leaving it on the burner for an hour, white fumes were still condensing in the receiver.I was running out of gas and had to turn it off.So , I never got to find out if any red oil distills over.
I usually cool the receiver by just placing it in a container of water.Using Ice+CaCl2 mixture might cause the red oil to condense.



The liquid to the left is acetone and to the right is yellow tinted acid.Although in the photo both look similar , to the naked eye there are some differences.The acetone is turbid while the acid is a clear transparent liquid.There is some white sediment in the acetone.
Not sure what it is or where it came from.It isn't visible in the photo.


The test tube with the acid has a small piece of gold in it.(It can be seen in the photo)
I'm going to leave it undisturbed for a few weeks and see what happens.

UPDATE: I had put a piece of gold into the acetone too .Now(after about an hour) it has turned greenish.



The gold comes from an old ring.It probably has high copper content. Maybe the sulphur of copper is being extracted

UPDATE: I haven't been able to replicate this experiment.

[k89]

Not sure if this is important..but I'm posting it anyway.

Here is a photo of the test-tube containing the acetone distilled off gold acetate (that turned green- photo in my earlier post)
A piece of gold metal has been sitting in this for two weeks.



There are no visible changes in the test-tube containing the yellow tinged acid and gold metal.

UPDATE: Better Pic

[Field]

Beauitful Evil,

Thank you for starting this thread which I found after doing a search for Gold Acetate and Alchemy. I am a member of Nick's conclave and I have produced Gold Acetate in solution. It is yellow colored with brown sediment at the bottom. Also it is kept in a jar and hanging on the lid of the jar there are a few drops of red liquid. I am interested in following this path in order to make the Philosopher's stone. Here are some pictures of the Gold Acetate, which I have found a relatively easy way to make. Would you please help me out with what I should do next as I am not familiar with this gold acetate path but just obtained the gold acetate by accident as a result of some of my experimentation and intuition. I look forward to sharing my results with the forum. Thanks in advance.

[k89]

I have produced Gold Acetate in solution. It is yellow colored with brown sediment at the bottom

Exactly how did you prepare the acetate?
The red liquid on the lid is interesting.

[Salazius]

Very nice indeed.
Did the acidity of the solution mixed the iron of the lid with gold to produce this redness?

Regards,
Salazius

[BeautifulEvil]

Guys and girls, I have had many a revelation on this particular process during my absence! Ah, where should I begin?

Even though it's been said that the copper/silver/gold acetate shouldn't produce anything other than radical acetic acid, in fact these do produce other products, just like the other acetate salts. This has been experimentally confirmed by k89. The major products are a milky acetone spirit, acetic acid, and an oil (must be distilled at high temperatures to obtain a decent quantity of this oil). The ratios and qualities vary between acetate salts.

However, the rectified acetone from this process should be digested. This will result in a very very lovely smelling product, and digestion should be continued until this sign appears. After the digestion a "graduated" acetone oil will float on top of a phelgm-like acetone layer. This oil will extract the sulphur from all the metals, and I believe the bottom layer of acetone will also (except its action is much slower and less aggressive). Why does this happen, and why is an oil produced? Well the acetone will contain small amounts of acetic acid, and during digestion this causes an ester synthesis to occur must faster than would have been possible with pure acetone. Interestingly enough, this process can be carried out with commercial acetone, and it will produce a slight layer of oil.

Either way, this acetone is the Philosophical Spirit of "Wine" (think Lully / Secrets of the Adepts). The acetone from this process will indeed extract the sulphurs from ALL seven metals, and it was the greatest secret in all of alchemy.

The acetate salts should be lightly calcined at 120F to remove any water remaining in the salt. This will make for a better distillation. Also, one should attempt to remove all traces of acetic acid before attempting dry distillation. The product is infinitely better I believe.

Exactly how did you prepare the acetate?

I believe it can be prepared using an oxide, hydroxide, or carbonate of gold. This is then added in proper ratios to a rectified solution of wine vinegar.

[Field]

Thanks for the reply everyone,

The way I got the golden vinegar solution was by taking Gold dissolved in distilled water, adding it to vinegar, and letting it putrefy. The solution turned from clear to golden and there was also a film or oil floating on the surface. Also over time the red drops formed as condensation on the lid. This may or may not have something to do with the iron in the metal lid. When I looked at it the other day there were no longer any red drops but instead a red earth on the lid and when I scraped it off it had a glassy appearance. During the process some of the paint on the lid got scraped off exposing the metal, and now more red earth has formed over this exposed metal. This new formation of red earth does not appear to be rust because it is not rusting the metal itself, just appearing on the surface. It seems to be something that is coming from the Gold Acetate solution.

The solution itself smells very sweet and the glassy red substance is very beautiful.

[BeautifulEvil]

Some interesting observations Field.

The way I got the golden vinegar solution was by taking Gold dissolved in distilled water, adding it to vinegar, and letting it putrefy.

How did you dissolve elemental gold in distilled water? It must have been a gold salt?

From what I've read, it seems to all revolve around the philosophical acetone. When it's added to various acids, the strength to extract sulphur from a metal is drastically increased.

[Field]

No it was not a gold salt. It was elemental gold dissolved in distilled water. And I didn't do it, an Alchemist friend of mine did and I don't know how he did it. But if anybody is interested in getting some there is a possibility I can help.

[k89]

Also over time the red drops formed as condensation on the lid.

Ferric acetate is reddish brown in solution form.
It is possible that some of the acetic acid in the gold solution reacted with the iron in the lid , but,I'm not sure if acetic acid is volatile enough to evaporate and condense on the lid.

This oil will extract the sulphur from all the metals

Did you see the picture I posted earlier.(The one with a red oil floating on it)
200 mg of gold digested in the acetone distilled of gold acetate ,left undisturbed for two weeks ,yielded a distinct layer of red oil on the surface.A drop of the oil added to water resulted in a beautiful iridescent film on the surface of the water.Within a few seconds the iridescence diminished.

[BeautifulEvil]

200 mg of gold digested in the acetone distilled of gold acetate ,left undisturbed for two weeks ,yielded a distinct layer of red oil on the surface.A drop of the oil added to water resulted in a beautiful iridescent film on the surface of the water.Within a few seconds the iridescence diminished.

Sorry, I didn't look at the image very close. That's really interesting though!
Didn't you say the acetone, when freshly distilled from the gold acetate, looks kind of milky? IF that's the case, then it would back up the claims of the alchemists which say their philosophical mercury is a milky white substance.

If you perform the experiment again, can you try digesting the acetone from the gold acetate distillation @ 40c for a few weeks?

[Sponsored content]