Re: Dry Distillation of Acetate Salts

[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.

[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)...