Dry Distillation of Acetate Salts

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Re: Dry Distillation of Acetate Salts

Post  Field on Wed Sep 03, 2008 8:34 am

Thanks for the reply k89,

That's a really nice picture you have of the red oil! So you are saying that you take the gold acetate dissolved in vinegar and when you distill it at the right temperature it produces acetone? Do you dissolve the gold acetate salt seperately as a dry distillation or do you do it with the vinegar too?

That's interesting about the irridescent oil forming too! It would have been interesting if you could have captured some Smile

As far as my experiment, I don't think the vinegar can be called acetic acid anymore because it has a very different smell. It has a sweet smell and it no longer is irritating to the mucous membranes like vinegar. It was only the vapors from the solution that formed the red drop on the lid. The lid is metal but initially it was covered with some kind of paint layer so if it has to do with the metal turning the drop red I don't see how when the metal was not exposed. I think the red is just a concentrated color of the Gold Acetate solution that is caused from a very slow and mild distillation occurring naturally within the sealed container, but now that the paint has been scraped off a little and the metal is exposed it definitely seems to be drawing some kind of solid red substance through the air above the solution.

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Wed Sep 03, 2008 12:46 pm

That's a really nice picture you have of the red oil! So you are saying that you take the gold acetate dissolved in vinegar and when you distill it at the right temperature it produces acetone? Do you dissolve the gold acetate salt seperately as a dry distillation or do you do it with the vinegar too?
Ah I know I'm not k89, but I believe I can answer your questions. The gold acetate salt should be made first. This salt should ideally be lightly calcined at 120F to remove trace water. As you know there may be small amounts of acetic acid residue present, and this should also ideally be removed. After you have the pure lightly calcined gold acetate you may proceed with the dry distillation.

I remember reading that the temperature should be slowly graduated and adjusted over many days to obtain the BEST products.

Use a retort and connect to it a decent size two necked RB receiver flask (heavy wall), one opening will be connected to the retort, the other will connect to a lower heavy duty one neck RB receiver flask (this should be kept cold throughout the dry distillation process). All the joints should be air tight, and it may be best to lute each joint.

Then start the distillation at 75F and slowly increase it to a few hundred F over the course of a week or so. In the end you will be left with the most volatile mercurial products in the second flask, and the other sulphurous products in the first flask. The volatile products will mostly be acetone.

EDIT: Also this should always be done in darkness, because gold salts are photosensitive and will readily decompose in presence of light or the sun (especially the sun). Life is nourished in darkness, but light is the destruction of life.


Last edited by BeautifulEvil on Thu Sep 04, 2008 11:16 am; edited 1 time in total

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Re: Dry Distillation of Acetate Salts

Post  k89 on Thu Sep 04, 2008 8:50 am

The gold acetate salt should be made first. This salt should ideally be lightly calcined at 120F to remove trace water. As you know there may be small amounts of acetic acid residue present, and this should also ideally be removed. After you have the pure lightly calcined gold acetate you may proceed with the dry distillation.

Yes that is how I did it.
Like i said earlier, gold acetate distilled on a gas burner (not sure of exact temperature) yields acetone whereas at low temperatures (<300 Celsius) it yields yellow tinted acid.

Use a retort and connect to it a decent size two necked RB receiver flask (heavy wall), one opening will be connected to the retort, the other will connect to a lower heavy duty one neck RB receiver flask (this should be kept cold throughout the dry distillation process). All the joints should be air tight, and it may be best to lute each joint.

I've used nothing more than a simple distillation unit.
But using two retorts would be the most efficient way of separating the products.


As far as my experiment, I don't think the vinegar can be called acetic acid anymore because it has a very different smell. It has a sweet smell and it no longer is irritating to the mucous membranes like vinegar. It was only the vapors from the solution that formed the red drop on the lid. The lid is metal but initially it was covered with some kind of paint layer so if it has to do with the metal turning the drop red I don't see how when the metal was not exposed.

Ah,this is interesting.
Have you tried using a glass/plastic lid instead of a metal one?
Could you elaborate on the process used in making the gold acetate?


It was elemental gold dissolved in distilled water.

Are you referring to colloidal gold here?

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Thu Sep 04, 2008 11:14 am

I've used nothing more than a simple distillation unit.
But using two retorts would be the most efficient way of separating the products.
Yeah, you may use a single retort and receiver flask. This results in all the products ending up in the single flask which may be separated again by a slow distillation of all the liquid in the receiver flask. I mentioned using two flasks because it's sort of easier to just collect the acetone separately from the others since it's the most volatile and will end up in the cooled second flask.

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ferric acetate

Post  k89 on Sat Sep 06, 2008 6:56 am

Ferric acetate on dry distillation gives a tinted acid too.
Not sure of the color.It is very faint. In my opinion ,it is tinted brown.
It is definitely an acid (bubbles with carbonates).
(Click to enlarge)


In the photo,the test-tube on the left contains the acid and the other contains common water.

After adding a few drops of water to the acid , it turned milky.
The acetic acid from gold acetate also turned milky when water was added.




Last edited by k89 on Tue Sep 09, 2008 4:00 am; edited 1 time in total

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Sat Sep 06, 2008 11:06 am

Ah, so it was the acetic acid which turned milky?

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Re: Dry Distillation of Acetate Salts

Post  k89 on Sat Sep 06, 2008 11:12 am

Ah, so it was the acetic acid which turned milky?

Yes

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silver acetate

Post  k89 on Wed Sep 10, 2008 11:09 pm

Silver acetate on dry distillation at 300 Celsius gives a nearly colorless acid.The acid has a very faint yellow tint.
So faint that I noticed the color only when I compared it with a test-tube of water.
This acid too turns milky white when water is added.

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Wed Sep 10, 2008 11:15 pm

Silver acetate on dry distillation at 300 Celsius gives a nearly colorless acid.The acid has a very faint yellow tint.
So faint that I noticed the color only when I compared it with a test-tube of water.
This acid too turns milky white when water is added.
Did it only give acid or did you also get acetone? Did it smell strange like all the others?

I'm glad you confirmed this with silver acetate! That was another suspicion of mine. Very good indeed. Can I ask if you've tried to produce a Stone from these? That would be on my list of "things to try next."

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Re: Dry Distillation of Acetate Salts

Post  k89 on Wed Sep 10, 2008 11:24 pm

Did it only give acid or did you also get acetone? Did it smell strange like all the others?

I've done the distillation at low temperature only and this yielded an acid.
At higher temperatures it may give acetone(similar to gold).I will be trying this soon.
The acid smells the same as all the other acids I've obtained by dry distillation.


Can I ask if you've tried to produce a Stone from these?
Not yet.
Working with acetates is very interesting.I need to learn more before attempting to make a Stone.

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Wed Sep 10, 2008 11:34 pm

The acid smells the same as all the other acids I've obtained by dry distillation.
Ah, so it's basically the same I'd assume. Maybe slightly different according to the particular bond potential between the metal and the acetate, but only slightly.

At higher temperatures it may give acetone(similar to gold).I will be trying this soon.
Have you approximate temperatures in which the acetone begins distilling over? Maybe we could compare the starting temperature, when the acetone begins coming over, to the various salts of acetate. I'd like to know which comes over at the lowest temperature. I have a suspicion it might've been lead acetate, but this is more of a poke in the dark (of course the decomposition temp of lead acetate is only 100C, much less than the others Wink). Can't wait to see how it goes.

Working with acetates is very interesting.I need to learn more before attempting to make a Stone.
I understand. I agree 100% with you, the acetate work IS very interesting. I need to get off my lazy butt and get to work. LOL

EDIT: Also I believe silver acetate is photosensitive, did you work in the dark? If this is the case, then I have to admit, it backs up the words of various alchemists "our work is to be done in the dark."

I would like to see what happens with mercury acetate, but as you can well understand, this would be quite dangerous! I can only imagine the horrible, life threatening, vapors. Mercury acetate begins to decompose around 179°C.

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Re: Dry Distillation of Acetate Salts

Post  k89 on Wed Sep 10, 2008 11:49 pm

Have you approximate temperatures in which the acetone begins distilling over? Maybe we could compare the starting temperature, when the acetone begins coming over, to the various salts of acetate. I'd like to know which comes over at the lowest temperature. I have a suspicion it might've been lead acetate, but this is more of a poke in the dark. Can't wait to see how it goes.

The acetone of gold distilled over only when I used a gas burner. It is a small burner that runs on butane and is used for cooking purposes.I'm not sure what temperature it produces.
From personal experience, I can say that lead and zinc acetates are the easiest to work with to get acetone.



Also I believe silver acetate is photosensitive, did you work in the dark?

I worked under artificial lighting.No sunlight fell on it.I think indoor lighting doesn't produce enough UV rays to bring about decomposition.

I would like to see what happens with mercury acetate, but as you can well understand, this would be quite dangerous! I can only imagine the horrible, life threatening, vapors. Mercury acetate begins to decompose around 179°C

lol.
I really wanted to try this but mercury is very costly here.

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Wed Sep 10, 2008 11:55 pm

I worked under artificial lighting.No sunlight fell on it.I think indoor lighting doesn't produce enough UV rays to bring about decomposition.
Would you mind testing this by taking a small amount of silver acetate in solution and taking it outside. Should decompose into elemental silver. It's unnecessary, but it's more of a personal curiosity.


lol.
I really wanted to try this but mercury is very costly here.
Quite understandable. Ah, you can obtain it from mercury sulfide (vermillion) if you distill it multiple times, you should have relatively pure quicksilver (I'm sure you knew this already, heh). Also, look for mechanical tilt switches, they should have a small glob of mercury inside - just break these open, and voila.

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Re: Dry Distillation of Acetate Salts

Post  k89 on Thu Sep 11, 2008 12:27 am

Ah, you can obtain it from mercury sulfide (vermillion) if you distill it multiple times, you should have relatively pure quicksilver (I'm sure you knew this already, heh).

I just found out that vermillion is available as sindoor here in India.
Maybe I can work with mercuric acetate after all....

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Thu Sep 11, 2008 12:33 am

I just found out that vermillion is available as sindoor here in India.
Maybe I can work with mercuric acetate after all....
Heh, if I were you, I would make a primitive retort out of iron/steel pipe. This will be much better than contaminating your glassware. Atleast, that's what I would do in your situation.

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Re: Dry Distillation of Acetate Salts

Post  Field on Fri Sep 12, 2008 9:35 am

"Ah,this is interesting.
Have you tried using a glass/plastic lid instead of a metal one?
Could you elaborate on the process used in making the gold acetate?"

I have not tried using glass or plastic yet but I will give it a shot once I get a distillation unit. With the gold acetate you just add the Aetheric Gold in Distilled Water to Vinegar, seal, and putrefy.

"'It was elemental gold dissolved in distilled water.'
Are you referring to colloidal gold here?"

It's not colloidal from what I can tell. The solution is actually clear but it has gold dissolved in it apparently

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Failure

Post  k89 on Fri Oct 10, 2008 1:37 pm

I've attempted to distill acetone out of gold and silver acetates several times in the past few days. Sadly , all of them have been failures. Only an acid distills off even at high temperatures.
This means that so far I've obtained acetone from gold only once.I'm forced to conclude that that must have been due to the presence of sodium acetate impurities.But it did extract a red oil from gold...

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Re: Dry Distillation of Acetate Salts

Post  BeautifulEvil on Fri Oct 10, 2008 5:38 pm

I've attempted to distill acetone out of gold and silver acetates several times in the past few days. Sadly , all of them have been failures. Only an acid distills off even at high temperatures.
This means that so far I've obtained acetone from gold only once.I'm forced to conclude that that must have been due to the presence of sodium acetate impurities.But it did extract a red oil from gold...
Hmm, that's actually kind of interesting. I was fairly surprised when I heard you obtained acetone from gold/silver acetate. I was also kind of surprised when you obtained it from copper acetate. These three are only supposed to produce a radical acetic acid. Atleast that's what the literature states.

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Zinc Acetate

Post  k89 on Thu Dec 18, 2008 11:56 am

A red oil condenses near the neck of the retort along with zinc oxide.
Acetone condenses in the receiver.
red oil:



After adding the zinc oxide sublimate to the acetone and heating gently, a reddish brown oil separates out.


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Philosophical and Unphilosophical - The Acetate Path

Post  raedotted on Thu Dec 18, 2008 2:20 pm

I am very glad to see an interest in the Acetate Path, and I have read all of the posts in this thread.. I tip my hat to you on attempting these rare experiments. What I see here is that there are several reasons for the failed attempts, and I would like to point out where Alchemy departs from modern Chemistry. Trying to separate out the physical actions of the alchemist in the laboratory from these interior connections, bridging the spiritual and physical realms, reduces it to common chemistry. Compounding and purifying materials through chemical processes is not going to get us anywhere in Alchemy. There is a misconception regarding Spiritual and Practical Alchemy. Refining the practice of practical alchemy, requires increasing ones understanding of the philosophy or theory of alchemy. Increasing ones understanding of the theory of alchemy requires work and prayer (Ora et Labora). So alchemy really is a double headed snake.

The experiments discussed here in this thread, are basically chemistry experiments only. The result is going to be different then if the experiment were carried out according to the philosophy of alchemy. The processes used in laboratory alchemy strive to capture and preserve the operation of subtle essences in a suitable vehicle all the way to their material analogs.

In chemistry, we take certain ingredients and combine them through a process to obtain a certain result. And it is always the same result whether I mix it or you mix it. In alchemy this is not always the case. There is a subtle something, which can influence the end result.

Materials obtained through commercial means which are compounded and purified through processes would be considered by alchemists to be Unphilosophical and are dead bodies only. So what is Philosophical? To have your materials be philosophically prepared means you must follow the philosophy of alchemy and realize you are working with the life force and consciousness of your materials as well as the body. Gold hydroxide bought at the chemistry store for example is a dead body only. You cannot extract Philosophical Mercury from these materials, hence you cannot prepare the Philosophers Stone this way.

I am familiar enough with the theory of alchemy to lead you on the right track. I won’t disclose the methods and I'm leaving out some details, as they must remain concealed from the puffers who wish to commercialize these preparations. However, I can provide direction to those who are interested. Write me privately if you would like to learn more. I am more than willing to help fellow alchemists.

Preferably the starting materials should be Oxides, Carbonates, Sulphides, and Sulphates. These should be native ores extracted right from the earth. So my first suggestion would be to start with at least 5 to 10 pounds of raw metal ore, and calcine it to the oxide. Preparing a metal calx requires powdering the ore, and calcining it to drive off the impurities. Next, I suggest preparing the Radical Vinegar from copper acetate first. I won’t for sake of the puffers disclose the method here. Once the Radical Vinegar has been prepared, one uses the Radical Vinegar to convert the metal subject (gold oxide, etc) to acetate. The resulting acetate is dry distilled slowly at first, and then the temperature is increased to about 400 to 700 degrees C. The resulting distillate contains three secret substances. Since they are secret I cannot divulge any more about them. If you would like to know about them, and how to work with them, I suggest looking to the 1450’s alchemist George Ripley’s ‘Liber Secretisimuss’ also called "The Whole Work of the Composition of the Philosophical Stone and Grand Elixir, and of the First Solution of the Grosse Bodies." which can be found from the RAMS library. Basically, you must separate out these three substances and work with them to purify them further, before recombining them in its new exalted form. In conclusion if you do not do these operations correctly, and without the proper attitude, you will only run into disappointment and you might even harm yourself. Best of luck Brothers and Sisters!

-Rae


Last edited by raedotted on Thu Dec 18, 2008 2:35 pm; edited 1 time in total (Reason for editing : proofing)

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Re: Dry Distillation of Acetate Salts

Post  theFool on Fri Dec 19, 2008 2:42 pm

A red oil condenses near the neck of the retort along with zinc oxide.
It seems you succeeded. A similar pic of the red oil condensing on the arm comes from Paracelsus college lab:


You can check now if this red oil dissolves gold.

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Re: Dry Distillation of Acetate Salts

Post  Illen A. Cluf on Fri Dec 19, 2008 3:59 pm

raedotted wrote:I am familiar enough with the theory of alchemy to lead you on the right track. I won’t disclose the methods and I'm leaving out some details, as they must remain concealed from the puffers who wish to commercialize these preparations. However, I can provide direction to those who are interested. Write me privately if you would like to learn more. I am more than willing to help fellow alchemists.

Hi Rae,

Thank you for your generous offer to those who wish to attempt the lab work. I wish I could pursue it, but I have limited lab space and only the basic distillation equipment. I'm very interested in what type of furnace you use for your work?

Thanks
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Furnace

Post  raedotted on Tue Dec 23, 2008 9:13 am

Illen A. Cluf wrote:
raedotted wrote:I am familiar enough with the theory of alchemy to lead you on the right track. I won’t disclose the methods and I'm leaving out some details, as they must remain concealed from the puffers who wish to commercialize these preparations. However, I can provide direction to those who are interested. Write me privately if you would like to learn more. I am more than willing to help fellow alchemists.

Hi Rae,

Thank you for your generous offer to those who wish to attempt the lab work. I wish I could pursue it, but I have limited lab space and only the basic distillation equipment. I'm very interested in what type of furnace you use for your work?

Thanks
Illen

Hi Illen,

I don't use a furnace for the Acetate Path, although you can. I use a hotplate that reaches about 500°C, and a saucepan filled with clean sand. If you were to use a furnace I would suggest making it from some inexpensive fire brick, put a metal grate on the bottom, and use coals or heat the bottom with a gas torch. In the instance a furnace is used, it is necessary to make a clay helmet, to direct the vapors into the recieving flasks. See the drawing below for an idea of how the furnace should look. This is from John French's Art of Distillation:



A large assay crucible is placed into the furnace containing the acetate salts, and covered with a clay helmet. The clay helmet has a hollow tube built into it which connects to the cooled receiver via a condenser. The remaining vapors are sent to a third vessel and finally led outside.

Using a hotplate (much simpler):

The flask is immersed 3/4 of the way in sand contained in a saucepan. The distillation flask is led to a condenser which connects to the second flask. The second flask is double headed and immersed in an ice bath. The second neck connects to a third flask (also double headed) which passes the volatile vapors through water via a glass tube. From there the vapors leave the third flask through it's second neck into a fourth flask (also double headed) containing charcoal. From there a plastic tube is led outside to release any remaining vapors.
After bubbling through the water any toxic fumes are passed through charcoal in the fourth flask. From there a plastic tube can be lead to the outside. This is the safest method I have found. Don't forget to prepare your materials philosophically!

-Rae

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Re: Dry Distillation of Acetate Salts

Post  Illen A. Cluf on Tue Dec 23, 2008 3:05 pm

raedotted wrote:I use a hotplate that reaches about 500°C, and a saucepan filled with clean sand.

Thanks Rae. I didn't realize that a hotplate could be used for that process. The ones I have seen do not quite reach that temperature, and do not hold close to that temperature very well. Once it reaches close to that temperature, it will click off and drop about 50 degrees or so before coming back on again, making the process very frustrating. The one you are using must be very good quality.

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Hotplate

Post  raedotted on Wed Dec 24, 2008 8:30 am

Illen A. Cluf wrote:
raedotted wrote:I use a hotplate that reaches about 500°C, and a saucepan filled with clean sand.

Thanks Rae. I didn't realize that a hotplate could be used for that process. The ones I have seen do not quite reach that temperature, and do not hold close to that temperature very well. Once it reaches close to that temperature, it will click off and drop about 50 degrees or so before coming back on again, making the process very frustrating. The one you are using must be very good quality.

Illen

Hi Illen,

I use specifically a Cast Iron Top Hot Plate, Remote control RC1900 model I bought for about $280 from Lab Depot Inc. They have a website by the same name where you can find this hotplate. It reaches 480°C maximum, and because it's cast iron you can use it with glass or metal vessels. You are probably thinking, "But you said 500°C?" and yes this is true, I did say that. Keep in mind however, the sandbath will absorb more heat.

Rae

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