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View Full Version : what not to do... sodium acetate



elixirmixer
05-31-2016, 01:12 AM
This is the first of a series of threads that i like to call "what not to do:"

ive been studying alchemy a long time but still feel like a beginner and in truth i am. Here is an account of my sodium acetate experiment, starting fro. all the mistakes i made trying to create the acetate (sad, i know) and then the huge list of mistakes i made trying to distill it.

here goes, first attempt to create sodium acetate: put a bunch of bicarb in a good quality pyrex jar. poured acid over it. it bubbled, i shook it up, opening the jar every 5seconds or so to let the carbon dioxide out so the jar doesnt explode. it dissolved, liquid went from white to clear, i didnt want to boil it because i did not want to decompose the acetate molecules (im going into alot of detail because i want to help other beginners save their time and money) ((decompose means when the kinetic energy of heat breaks apart the chemical bonds of the molecule.))

but i got impatient... after staring at an evaporating dish for five minutes, i chucked in on the stove. cooked it until all liquid was gone, and my fears had come true, a seemily 50% of the product had decomposed into what i believe was probably lye. still had abit of bicarb smell and taste aswell as a bit on salt and vinegar chips (the taste we are looking for)

so i called in the help of my chemical engineer friend who worked out the proper reaction equation and gave me the 1:1.4 ratio of acid:bicarb.

so i tryed again. 289mls (ish) of acid. 420g of bicarb. mixed it ALL together, is softly bubbled away.... i know what your thinking... "you pored 300ml of 99% acetic acid straight onto bicarn and it ""slowly bubbled"".... Yes. it slowly thickened while mildly bubbling, eventually going quite hard in the jar. i needed to get it out so i reluctantly poored some water in the jar to dissolve it...
big mistake.... it seems that water REALLY catalyses this reaction. frothed out of control and created a mess so large that ive got people coming over today to clean it up because i cant be bothered with it.

THIRD ATTEMPT!: 300mls of acid (slightly more than recommended by the ptofessional) 400g of bicarb (slightly less) and put it in a nice wide mouthed glass dish. gave it a good stir ebery half hour until it set. hard as a rock in the morning, but quite succeful. tasted like salt and vinegar with no bicarb flavour.

next day i took to it with a hammer and chisle, well a hammer and butterknife actually, and broke it into small enough pieces to get into a 1ltr flask.

so here's where the real stupidity begins. my heating mantle is not a bowl, it doesnt full enclose the flask like some others often do, so 400g was far too much to have in the flask, the bottom went through transformation while the top layer hardened and peeved me off. then elixirmixer made a pathetic rookie mistake, and poored some distilled water into the flask (while still boiling) to try and dissolve the top layer to go to the bottom.

at first it seemed to do well, while not completely successful, some of the top layer did sink into a better position. but the room temp water cracked the flask pretty badly. if your as poor as i am, youll understand why that is not an ideal situation.

round two of the acetate dry distillation: clean flask, 100g of sodium acetate. locked the distilles water in a cabnet and turned on the heat full blast. another note of interest, pigtail condensers dont seem to enjoy being used on their side. it causes a weird pulsing suction effect which mixes your products while distilling which makes it harder to distinguish whats coming over and when.

So, this happened: bit out cleary-yellow liquid, with bery fine traces of red oil, followed by some very cool looking 'heavy smoke' white in appearance. the smell is weird, i put my gas mask on.. (okay maybe im poor cause i blow to much money on equipment).. then a fairly dark golden amber liquid, with relativly more red oil.
i really didnt get much red oil from 100g of acetate. robert bartlett said that he found that from the ~50mls of menstruum he obtained, the red oil only contributed 3.5%

NOW THE COOL PART! So i wanted to see what this menstruum would do to silver.. used bolt cutters to cut a slice of silver from a coin and dropped it in the product. The red oil grabbed hold of the silver, at least, 70% ish grabbed hold and whe i woke up this morning, i noticed some very light corrosion on the silver coin and also, the oil that had grabbed hold had now 'taken' what it wanted and fell away from the silver!

HOW COOL IS THAT!!?

elixirmixer
05-31-2016, 02:25 AM
Also, while cleaning up today i noticed that this distillation created what appears to be pure sodium metal on the bottom of the flask, the flask it self has bubbled in a ring around the bottom. im not sure if this is a result of thw sodium reacting with the silica under heat or weather its because i bought cheap crap from china. either way, another flask bites the dust!

theFool
05-31-2016, 06:20 AM
Your post stirred some thoughts to me. I have tried this experiment once, what I got mostly was acetone. This fraction of the distillate (acetone) is what Bartlet uses to do "extractions". Probably you are the first person I see to use the red liquid, (the "menstruum foetens") to do an extraction. In my opinion your way is closer to the old alchemical writings.

Some other questions:


a seemily 50% of the product had decomposed into what i believe was probably lye Can you be sure that it produced lye? If yes it would be a novel method to obtain lye from soda. But I doubt it is lye.


this distillation created what appears to be pure sodium metal on the bottom of the flask Again, this would be a novel way to produce sodium. I strongly doubt it is sodium in there but who knows. When you mix it with water does it produce hydrogen bubbles? Usually it bursts into flames when it comes in contact with water, you would have noticed it when washing it out.

Oh, and welcome here! I like your hands on approach to alchemy :)

elixirmixer
05-31-2016, 07:27 AM
Can you be sure that it produced lye? No I cannot be sure, in fact on reflection it is probably unlucky, but is certainly possible. Assuming the boiling DID decompose, and assuming that the vapor pressure of acetic acid allowed it to distill off before the water... nevertheless it was most likely just a poor combination of acetate, and un-reacted bi-carb... or something, nothing special I don't think.
I strongly doubt it is sodium it really looks like sodium, bit of a fix bit I was not able to demonstrate the 'pop' test to my friends. Does sodium oxide react the same way?

elixirmixer
05-31-2016, 07:30 AM
I'm not sure sodium bursts into flames unless it has an ignition source for the hydrogen. I know potassium does, sodium just fizzes and dance's around on top of the water (at least thats what I saw on YouTube today)

Ghislain
05-31-2016, 11:41 AM
Sodium metal self ignites.

Ghislain

theFool
05-31-2016, 06:59 PM
I'm not sure sodium bursts into flames unless it has an ignition source for the hydrogen. It does when it is in bigger chunks.


sodium just fizzes and dance's around on top of the water (at least thats what I saw on YouTube today) Question is, did you see it in your glassware?


Assuming the boiling DID decompose, and assuming that the vapor pressure of acetic acid allowed it to distill off before the water... nevertheless it was most likely just a poor combination of acetate, and un-reacted bi-carb... or something, nothing special I don't think. it really looks like sodium, bit of a fix bit I was not able to demonstrate the 'pop' test to my friends. Does sodium oxide react the same way? I don't have experience on how sodium oxide reacts with water. But, from wikipedia we find that:


Alternatively, sodium carbonate can be heated to 851 C, producing carbon dioxide and sodium oxide. Na2CO3 → Na2O + CO2

And:


At 208 C, sodium ascorbate will decompose to furan derivatives and sodium oxide. Probabaly you didn't reach 851 C (it would melt glass) but since sodium ascorbate decomposes to sodium oxide .. it is not at all impossible that sodium acetate does something similar.

theFool
05-31-2016, 07:23 PM
According to this publication ( http://jcsp.org.pk/ArticleUpload/2208-9977-1-CE.pdf ) you probably end up having only sodium carbonate after the destructive distillation.

elixirmixer
05-31-2016, 07:56 PM
It does when it is in bigger chunks.

Question is, did you see it in your glassware?

I don't have experience on how sodium oxide reacts with water. But, from wikipedia we find that:



And:

Probabaly you didn't reach 851 C (it would melt glass) but since sodium ascorbate decomposes to sodium oxide .. it is not at all impossible that sodium acetate does something similar.

The glass did melt although I doubt my little 600watt mantle could get that high. Acetate decomposes a lot lower.

Don't think it's carbonate, doesn't look, smell or behave like it. I might pH test it in the morning and see what we get there... it looks exactly like pure sodium, but doesn't behave as spectacularly.

I'd also like to add for any beginners reading, I had assumed (incorrectly) that acetic acid was pretty mild. It has since been brought to my attention that I've been exposing myself to a potentially very harmful chemical. Don't be a lazy jackass like me, wear your PPE!

elixirmixer
06-07-2016, 12:34 PM
So just an update. Threw a bit of copper into the mix. The red oil seems to enjoy 'hugging'the copper even more than the silver. I use the term hugging because I'm not sure I see much corrosion. What would be a really cool experiment would be to heat up a piece of metal, and plundge it into Thia menstruum. Flames aside, I'd love to see what the red oil does to hot metal's.

Still haven't drunk it, or bought a guinea pig.

I did lick the oil, didn't die.

elixirmixer
06-11-2016, 01:43 PM
Another update. Threw in a piece of copper. Same thing as with silver. Threw in a neyodinium magnet, the oil wasn't really interested in this one.

BUT the big thing is: few drops fell from the condenser I left sitting there (I don't usually clean up after experiments till the whole lab is trashed) the drops fell on my iron /steel retort stand. It are through the paint and corroded the plate!!!! Thia menstruum seems to work well on iron. Next time I make it.. I'll try making a torture of iron from the foetens.