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Offline Frater EIE

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Carbonate salt?
« on: July 25, 2022, 10:03:52 AM »
Hey all
I have a random question. Let's say I take an organic compound -we'll say a citrate for example- and we destructively distill it (pyrolysis) and obtain acetone and a mixture of phenolic compounds (tar?). Let's say we then gently calcine these compounds until we obtain a white salt. Can anyone tell me what this salt is?

Offline Hunter2

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Re: Carbonate salt?
« Reply #1 on: July 25, 2022, 11:10:28 AM »
If you used Calcium citrate for this then calciumcarbonate will remaining, depending of temperature also calciumoxide would be possible.

Offline Frater EIE

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Re: Carbonate salt?
« Reply #2 on: July 25, 2022, 11:38:49 AM »
Hunter2, supposing it was calcium citrate, wouldn't the calcium have stayed behind in the boiling flask during the initial pyrolysis? Remember, the salt in question is from the calcination of the phenolic compounds recovered from pyrolysis, not the citrate itself

Offline Hunter2

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Re: Carbonate salt?
« Reply #3 on: July 25, 2022, 11:40:30 AM »
What was the first product what got thermolysis. The organic will distilled and thermolysed. Inorganic will be left.
« Last Edit: July 25, 2022, 12:04:55 PM by Hunter2 »

Offline Frater EIE

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Re: Carbonate salt?
« Reply #4 on: July 25, 2022, 02:13:29 PM »
It would be iron citrate destructively distilled to form, water, acetone (I think... or some other volatile spirit) and a red oil that is mostly a mixture of phenolic compounds. Then those compounds are gently calcined over a long period of time. Gently is the key word here. Let's say that the boiling point of the compounds is never reached. A weird question, I know

Offline Hunter2

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Re: Carbonate salt?
« Reply #5 on: July 25, 2022, 02:15:47 PM »
Then a iron compound will be left. But iron compounds are yellow to brown and not white.

Offline Frater EIE

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Re: Carbonate salt?
« Reply #6 on: July 25, 2022, 03:14:38 PM »
No, I'm not talking about the calcination of the iron oxide.
Step one: iron citrate is dry distilled. From the breakdown of the organic citrate compounds first water vapor lcomes over the still head and then a white fume, and then finally an orange-red fume. The white fume condenses as a volatile spirit (acetone I think) and the red fume condenses as a red oil and is a mixture of mostly phenolic compounds. This mixture is what I'm asking about, not the iron left over. Forget the iron. It was left behind in the boiling flask. The citrate was destroyed and now the water, the spirit, and the red oil is in the receiving flask.
The second step is to separate out the red oil from the rest of the distillates and gently calcine it (using low temperatures) until it becomes a white salt. Does anyone have an idea of what this salt might be?

Offline Hunter2

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Re: Carbonate salt?
« Reply #7 on: July 25, 2022, 03:19:39 PM »
There will be no salt, maybe a white residue. Salts are made by a metal or ammonium ion and an anion of an acid. There is no nitrogen compound in your mixture so you can also erase this.

Offline Frater EIE

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Re: Carbonate salt?
« Reply #8 on: July 25, 2022, 03:37:54 PM »
Hmm, curious. Thanks for your answer. I'm doing a research essay on historical alchemy. It appears as if the alchemists were able to get some kind of white salt-like substance from these phenolic compounds, and that it was of essential importance to them.
What if, rather than calcining, we were to separate out from these oils the acetone-soluble portion in cycles by dissolving and decanting, until the acetone is no longer tinged by the oils, and then repeat this with the water-soluble portion? I know this makes things complicated and it's likely that experimentation is needed, but I was sincerely hoping the answer might be able to be arrived at by someone with an education in chemistry (unlike myself).

Offline DrCMS

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Re: Carbonate salt?
« Reply #9 on: July 26, 2022, 12:31:01 PM »
Step one: iron citrate is dry distilled.

How was the iron citrate prepared and purified?

From the breakdown of the organic citrate compounds first water vapor lcomes over the still head and then a white fume, and then finally an orange-red fume. The white fume condenses as a volatile spirit (acetone I think) and the red fume condenses as a red oil and is a mixture of mostly phenolic compounds.

Acetone I can see as a possible product from citrate but not sure how this would give a phenol or other aromatic compound.

The second step is to separate out the red oil from the rest of the distillates and gently calcine it (using low temperatures) until it becomes a white salt. Does anyone have an idea of what this salt might be?

What does calcine at low temperature mean?

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