arkoma
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Calcium Acetate dry distillation
Been saving eggshells and soaking in vinegar til I had several ounces Calcium .Acetate. Put 20gm in my little 250 sidearm disty rig and never got any
acetone but did get thick white fumes that ended up clogging the top of the worm in my graham condenser. Had an aluminum foil tent around that I
removed for clarity. Sorry about the picture quality. Any ideas what I have? GAA?
 
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NEMO-Chemistry
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Isnt that the dry calcium Acetate? Then you dry distill that for Acetone?? WARNING i been using Toluene today  .
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aga
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The stoi says you should have ended up with about 7g of acetone and 12g calcium carbonate.
Given that the CaAc decomposes at 160 C and acetone boils at 56 C, my guess is that it was a bit of a frisky reaction, blowing both the CaAc and
calcium carbonate all over the place.
Was it a bit like vesuvius ?
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NEMO-Chemistry
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Quote: Originally posted by aga  | The stoi says you should have ended up with about 7g of acetone and 12g calcium carbonate.
Given that the CaAc decomposes at 160 C and acetone boils at 56 C, my guess is that it was a bit of a frisky reaction, blowing both the CaAc and
calcium carbonate all over the place.
Was it a bit like vesuvius ? |
Actually i change my answer to what he said ^
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aga
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That kinda thing just racks up the post count rather than explore any chemistry.
Weren't you busy taking photos of a whole series of distillations or something, which we'll all see posted shortly ?
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NEMO-Chemistry
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| Quote: Originally posted by aga | That kinda thing just racks up the post count rather than explore any chemistry.
Weren't you busy taking photos of a whole series of distillations or something, which we'll all see posted shortly ? |
Shit, ok i guess i better go do it, i put it off long enough! first pic of set up in around 1 hour.
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aga
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Take your time and do the Science right, also the amazing photos, plus the tables of data that come out of the scientific process.
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arkoma
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Being back to work is kicking my but but I got home last night and took pictures and did one rudimentary test.
Excuse the picture quality, all I have is a junky old phone as a camera.
This picture is of the side arm where this stuff actually crystallized
Sidearm outlet
Solid mass stopping up my Graham Condenser. 14/20 joint.
Remainder in flask. Bottom is charred looking so evidently a lot bit of organic material is contaminating my CaAcet, but that is no surprise due to
the fact all I did before xtalizing was boil and filter the solution to precipitate out most of the proteins.
Anyway, I dug some out of the top of my Graham and dissolved 0.1gm in 2ml water. It dissolved pretty easy and the solution pH'ed to 9. The solid has
an acrid ammonia like smell.
*edit* @ aga, no Vesuvius or anything else untoward while heating. Some melted and formed a dark yellowish liquid and from this the white fumes
evolved.
I really need to quit buying moonshine supplies for a month and get a decent camera for closeups *sigh*
[Edited on 12-28-2017 by arkoma]
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
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ninhydric1
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arkoma, did you try recrystallizing the calcium acetate? It might've allowed a smoother, cleaner destructive distillation.
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Magpie
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If you have material crystallizing in your condenser you don't need a condenser. But if you use one then use air as the coolant.
The single most important condition for a successful synthesis is good mixing - Nicodem
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