Removing ethyl acetate by room temp fractionation

[raketemensch]

Sorry, I am either missing the obvious in the photo or am taking a wry remark seriously.
What process is the photo depicting?

Plain old airing out.

It's actually what the OP is trying to do but they want to speed it up.

Ah, what I often do for that is remove the lid part of a 2-piece mason jar, drop a coffee filter over the top, and screw the other part of the lid on.

[FuelMaker]

Just tossing out an idea, what about pumping it through a fine mist sprayer into a uprising stream of air and condensing the results on the walls of a cold trap like a highly chilled pipe - something like a pipe coming up through a bowl filled with azeo ethanol and dry ice. The mist droplets would have a huge surface area to react with the air.

Or doing it in batches by spraying in a sealed container.

I know they make stainless sprayers, we've got one at work.

Potentially explosive though.

[Tomb]

Sorry, I am either missing the obvious in the photo or am taking a wry remark seriously.
What process is the photo depicting?

Plain old airing out.

It's actually what the OP is trying to do but they want to speed it up.

Ok, is the cloth (or paper towel) acting as a wick or just to prevent bugs from getting in?
(Again probably overthinking this)

Tom

[Bagasso]

Ok, is the cloth (or paper towel) acting as a wick or just to prevent bugs from getting in?
(Again probably overthinking this)

I'm not Shadylane but, since it looks dry, I'm pretty sure it's there to keep out the bugs.

[manu de hanoi]

oh my god , you remove ethyl acetate by adding an alcaline to the stripped alcohol.
It breaks the ester into ethanol and acetate

it's hard to find food safe soda
so baking soda can be used (also avail as antacid)

[still_stirrin]

...you remove ethyl acetate by adding an alcaline to the stripped alcohol.
It breaks the ester into ethanol and acetate.

It's hard to find food safe soda, so baking soda can be used (also avail as antacid).

Yep...I just did this with a (7 liter) run of feints.

I put 2 tsp. sodium carbonate (I made this by baking baking soda in the oven at 250*F for two hours) into the boiler and ran it with the potstill head. It cleaned up the ethyl acetate nicely. It also gave me opportunity to pull the fores and heads again too.

The hearts smell and taste great, and when I got to the tails, the proof dropped very quickly too. A great method to salvage the feints.
ss

[Bagasso]

oh my god , you remove ethyl acetate by adding an alcaline to the stripped alcohol.

But this also gets rid of other esters you might want to keep.

[engunear]

still_stirrin, why did you bother with the bi-carbonate to carbonate conversion?

But its a great idea for making clean alcohol for gin and vodka base where you don't want esters. And so friggin obvious, once you know it. The more you can reduce things to the set of alcohols with their regular lineup of boiling points, the better a good column will pull them apart.

[jb-texshine]

Shadylane:

Sorry, I am either missing the obvious in the photo or am taking a wry remark seriously.
What process is the photo depicting?

Tom

That would be a rag or some such in the mouth of a jar to allow heads components that slipped by your cuts process to air out naturally and keep the bugs out at the same time. In the event of zombie apocalypse it doubles as a Molotov cocktail.

[engunear]

Back to carbonate vs bicarbonate, carbonate is more basic, which is probably good. But the bicarb to carb conversion happens even in hot water, so the additional step seems pointless. So if bicarb were added, the carbonic acid gets liberated as the pH rises which provides it for ethyl acetate conversion as the solution becomes more basic. Chemistry is not my strong suit, so am I missing something?

I'm gonna test this with a litre of stinky heads in water and a fractionating column set to 100% for a bit, if it comes out clean then thats a definitive result. This is the acid er basic test.

Just a comment also about detecting ethyl acetate, smell is really unreliable, especially from one day to the next. I have a jar with a wick in it as per the pic, but whatever happens I won't trust the result. What is needed is a second jar that is sealed, and a double-blind experiment comparing the two. Sounds like a lot of work, but there are so many ways the mind plays games. Recently, my Dad made some whiskey with a store-bought flavour and sugar vodka. I was pretty down on it. But later I tried some when I didn't know what it was, and found it a lot harder to criticise. The mind is not what it seems.

[engunear]

Experiment with carb soda inconclusive ... but ... probably did not wait enough ...

http://homedistiller.org/distill/dtw/strip" onclick="window.open(this.href);return false;" rel="nofollow

[der wo]

Carbonate vs bicarbonate:
Somewhere here I read, you need triple the amount of bicarb as carb for the same effect. I found out at room temp 15g of bicarb solve much less in 1l low wines than 5g of carb. So I prefer the carbonate.

[Bagasso]

I found out at room temp 15g of bicarb solve much less in 1l low wines than 5g of carb. So I prefer the carbonate.

Solubility of bicarb in water is 96g/l at room temp (20ºC). If you have <40%ABV low wines there should be enough water to dissolve 15g of bicarb.

Maybe the change in pH is causing something else to fall out of solution.

[der wo]

Try it. If you put it in, it immediately forms snowflakes.

Edit: I asked wikipedia:
Bicarb: 96g/l
Carb: 217g/l
Carb is way better soluble and you only need 1/3 of that. So, if you have this problem with bicarb, try carb.

[Bagasso]

Try it. If you put it in, it immediately forms snowflakes.

I always get snowflakes no matter what I use. Then again I go past 10 pH.

[der wo]

Maybe the change in pH is causing something else to fall out of solution.

But what could it be in a stripped BW? I think it's the bicarb. With shaking and time 5g/l carbonate get in solution, 15g/l bicarbonate not, in my expierience. To put it on a radiator helps. But perhaps it's not necessary, perhaps it's ok, when it gets in solution while distilling.

[Bagasso]

But what could it be in a stripped BW?

There is stuff in there. I have used sodium hydroxide pre-dissolved in water, so not a solubility problem, and I get white or blue fluffy stuff falling out every time.

[der wo]

Ok, when I put carb or bicarb into low wines it solves immediately and something different falls out immediately?
I tried it just again and no, I cannot believe your theory. It looks simple: The carb falls in the liquid and forms flakes. That's all.
I did a video of that, but unfortunately it's not possible to post a mpeg.

[thecroweater]

Ok, when I put carb or bicarb into low wines it solves immediately and something different falls out immediately?
I tried it just again and no, I cannot believe your theory. It looks simple: The carb falls in the liquid and forms flakes. That's all.
I did a video of that, but unfortunately it's not possible to post a mpeg.

You could upload to youtube and post that though

[Bagasso]

I tried it just again and no, I cannot believe your theory. It looks simple: The carb falls in the liquid and forms flakes. That's all.

That's ok, it's just an idea.

I don't really watch it all that close but I do recall that the bicarb disolves and is gone after letting it sit for a while. What I see fall out is not bicarb flakes or grains but a softer looking layer. Like a soft cloud that settles to the bottom of the bottle but that is after letting sit for even longer.

[der wo]

Ok, I uploaded the video. PLEASE, if it is not safe what I did, if anyone can see, this video is dangerous for my anonymity, warn me ASAP!
https://www.youtube.com/watch?v=Y9zNvOs ... e=youtu.be" onclick="window.open(this.href);return false;" rel="nofollow

[thecroweater]

Not as far as I can tell, seems fine

[jb-texshine]

Now cap the jar and shake vigorously.

[der wo]

Shaking has no effect. But two hours on a radiator (I think it has 35°C after that), then shaking and everything is solved.
It was 5g carbonate in 1l around 40%. 15g bicarbonate would not solve in 1l 40% 35°C.

[Bagasso]

Are you testing the pH? That is what it is really about. That is probably why I never paid much attention to whether it dissolved or not.

Looking at 500ml with 15g bicarb in it. Did have a good amount settle. Don't know if it will dissolve with time but my pH meter reads 9.44 so, who cares?

[der wo]

Good idea. I measure pH 11! Only test strips, but good quality ones. What do you think about? Is that too high? Feints without carb/bicarb I measure pH 4.

Edit: the pH 11 is with solved carbonate (warmed on a radiator).

[Bagasso]

Good idea. I measure pH 11! Only test strips, but good quality ones. What do you think about? Is that too high? Feints without carb/bicarb I measure pH 4.

I don't think it is too high. That is what Manu advises in this post
pH 11 at 30º for 1 to 3 days.

ETA: Yes bicarb is only supposed to bring pH up to around 8.4 when saturated. I had forgotten that that is why I actuall switched to calcium hydroxide. Of course it also doesn't seem to dissolve completely. Last time I used 1/4tsp in a liter some settled out but pH went past 12.

[der wo]

Thank you. Interesting lab analysis results manu had. Muuuch less Esters and Aldehydes with high pH. I didn't think, it's such effective...

[engunear]

Well my 5l with quite a lot of carbonate (arrrrghhhh what precision!) in the sun for a week still stinks. This is the smelly heads in between the totally vile heads and the the good booze from a column, so its rich in ethyl acetate without having too much of the other evils.

Next experiment is with aquarium air pump.

Reading on this ... the net (which is always right) seems to be saying that a strong acid or a strong base will reverse esterification. So HCl followed by bi-carb neutralization (so it goes to NaCl), or NaOH might be the shot.

Not quite room temp fractionation. But what do they say? "a nod is as good as a wink to a blind man".

[Kareltje]

I do not really understand the problem.
The heads contain not only ethylacetate, but also methanol and other nasty ingredients, so removing the ethylacetate is solving only a (small) part of the problem.
And more important: alcohol is, after water, the cheapest ingredient of a drink. It is easily made by fermenting sugar and the loss of ethanol is hardly a problem or a large cost. Much more interesting is the production of volatiles that contribute to the taste of a spirit. And these can be found mostly further in the distillation process.
When you fear the loss of alcohol in the heads: just add sugar to the mash to compensate for this loss.