blogfast25
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A Nail Polish Remover Still...
I needed some relatively pure and dry acetone for my experiments with zirconyl chloride and a pharmacist in town seemed to be the only one having
some: 50 ml for the princely sum of $1.19 (only pharmacists can get away with this kind of extortion!) Considering a no frills acetone based nail
polish remover costs about £1.25 for 150 ml, I decided to try and distil off the acetone with a quickly cobbled together still. Rarely has a so
quickly conceived experiment worked so well for me...
The still (shown below in operation) is made of 2 empty vinegar bottles, washed properly, a piece of black, hard PP pipe, 1" diameter, about 3 mm wall
thickness and 220 mm long and a defunct aquarium siphon. One bottle serves as the reboiler, the other as condenser/distillate recipient. As luck would
have it the bottle cap fitted really snugly inside the pipe so I drilled a large hole in it and with some teflon tape the pipe/bottle form a tight
seal and stiff joint and the pipe can simply screwed onto the reboiler.
At the bottom of the pipe, just above the drilled bottle cap I screwed in three self tapping screws, providing a simple mesh. The pipe, now a column,
was the filled with small marbles (less than 1/2 inch). Rashig packing would be better of course but when given lemons, make lemon juice...
Again luck came to my help for the column head in the form of an aquarium siphon, the bottom end of which happened to fit like a glove over the top
end of the column, using a bit of teflon tape as sealant. The rest of the corrugated thin PE hose form the condenser/distillate pipe.
Finally a pinprick was made in the column head and a thermocouple carefully needled through, the elasticity of the PE providing a simple but adequate
seal.
Heating to the reboiler is provided with a water/steam bath.
The condenser bottle was sat inside half a 1.5 l pop bottle, immersed in iced water.
Reflux is provided by natural cooling: in essence it's a primitive Vigreux column.
Total assembly time? About an hour...
After a quick test for air tightness, it was testing time! I chose Boots 'expert conditioning nail polish remover', £1.25 for a bottle of 150 ml and
bought two.
Its listed ingredients are acetone, water, perfume, Prunus armeniaca kernel oil, panthenol, propylene glycol, alpha-isomethylionone, denatonium
benzoate, benzyl alcohol, limonene and linalool. At a glace acetone would appear to be the lowest boiling of the mix (azeotropes cannot be excluded of
course). It's a cheerful amber colour.
Prior to the first run with a 150 ml, boiling point of the nail polish remover was established to be 60.5 C.
Starting with boiling water at t = 0, temperature in the still head reached 57.1 C in about 10 min and distillate started coming over at a little
faster than 1 drop per second. There was clearly reflux flowing back into the reboiler, at a glance slightly faster than distillate was gathering in
the condenser. Temperature remained stable at 57.1 to 57.0 C. The BP of pure acetone is 56.5 C, it forms no azeotrope with water. I need to check
calibration of the thermocouple bur here we seem pretty close to the BP of acetone. The distillate, the first 10 ml or so discarded, was perfectly
clear. The liquid in the reboiler became more orangey and stared also to cloud over. After about 50 min the level of liquid in the reboiler started
getting rather low and distillate came over more slowly too, so I stopped there. About 50 g of distillate was obtained.
First run: the clear distillate can be seen gathering.
The apparatus had held up very well but there was some leakage from the bottle/column joint. I tried to remediate this for the second run with some
teflon tape on the bottle head but it made matters slightly worse. But this is nothing a bit of proper sealant can't solve: teflon isn't very elastic.
No acetone could be smelled during the distillations.
First run: shot of head temperature:
The second run went very similar despite slightly more leakage. 60.6 g of clear distillate was obtained with head temperatures this time ranging
between 56.4, up to 56.9 and then back to 56.7 C.
Reflux could be increased by running a couple of brass pipes, cooled with water running through them, through the top of the column.
All in all a very pleasant experiment...
[Edited on 8-6-2010 by blogfast25]
[Edited on 8-6-2010 by blogfast25]
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bbartlog
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Remembering my own mishaps distilling with plastic gear, I get nervous looking at your setup (though I'm sure it's fine for 60 deg C). Anyway, well
done - too bad acetone is not a common item of commerce where you live; they sell it in five liter cans (~ USD $36 if I recall correctly) at the Home
Depot here in the US (though the design of the can is atrocious for actually dispensing the acetone...).
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hissingnoise
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Nice bit of improvisation blogfast - not having seen the second v. bottle at first, I marvelled at acetone apparently sitting quietly in a plastic
Coke bottle. . .
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blogfast25
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Quote: Originally posted by bbartlog  | Remembering my own mishaps distilling with plastic gear, I get nervous looking at your setup (though I'm sure it's fine for 60 deg C). Anyway, well
done - too bad acetone is not a common item of commerce where you live; they sell it in five liter cans (~ USD $36 if I recall correctly) at the Home
Depot here in the US (though the design of the can is atrocious for actually dispensing the acetone...).
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Thanks for your concern but I'm a very careful home chemist. The low temperature of the distillation is of course what makes this safe, as well as
using a steam bath and not direct flame as a heat source...
The column is 1" PP pipe BTW, not 2" as was initially indicated. It's been edited now...
As regards obtaining pure acetone here (apart from the pharma grade), I'm sure that's possible: several small companies nearby probably use it. But I
only need small quantities: another distillation of 300 ml of NPR, this time without leaks, should keep me in acetone for weeks...
[Edited on 8-6-2010 by blogfast25]
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not_important
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Nicely done hack.
If you haven't read it, this thread may be of interest http://www.sciencemadness.org/talk/viewthread.php?tid=4488
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blogfast25
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@ not_important:
No, I hadn't seen that seen that thread but had been wondering how to dry acetone, other than by distilling. Also, how to determine moisture other
than by Kjeldahl, is there something something simple and approximate? Have computer, will search...
Ironically for my drying of ZrOCl2 purposes, 100 % dryness is probably not even required but it would be interesting to see the distillation of K2CO3
dried NPR or to dry the distillate with K2CO3 and re-distil.
This afternoon I'm testing a few mods to the still, with a 300 ml batch of Boots' NPR...
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blogfast25
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Another 300 ml distilled but this time small a problem occurred: with a 300 ml charge the boiling behaviour was very erratic, with large 'outbursts'
of boiling followed by periods of 'quiet'. At one point a large gust of liquid and bubbles shot right through the column and the cooler tube and into
the distillate bottle! I wrote "a small problem" but this kind of thing could be catastrophic at larger scale... 
All NPR was recovered and split back into 150 ml quantities. Both were distilled without problems, the second one with added boiling stones (some
ceramic chips from a broken crucible): boiling was much more regular and vigorous. Head temperatures hovered around 57.0 C in both distillations...
I'm surprised that a low boiling multimix like nail polish remover would show erratic boiling, could it be that the doubled hydrostatic at the bottom
of the boiler bottle was preventing smooth boiling?? It'd be interesting how the distillate, e.g. after drying with Na2CO3 (I've no K2CO3), would
behave...
This time no leakage at the bottom but small leakage at the top occurred. I'll now not be modifying the still any further until I need some more
acetone. Then I'll fit some reflux in the head: I've got some RC plane brass fuel pipe with matching silicone tubing that's just perfect for the job!
On top of the 'bottom end' of the NPR floats a clear, oily substance: maybe the apricot oil and some other components whose solubility limit was
exceeded?
[Edited on 9-6-2010 by blogfast25]
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rrkss
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The erratic boiling is caused by superheating of the organic liquid followed by rapid formation of gas as the superheated liquid boils and returns to
its boiling point. This is exactly why organic chemists add pourous boiling chips to their flasks. These chips contain millions of little air
bubbles which allow for a smooth boiling.
The phenomenon you experienced is known as bumping.
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blogfast25
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Bumping, that's the term I was looking for... thanks!
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zed
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That appears to be a gas stove. Distilling acetone is no big deal, but I wouldn't fancy doing it with an open flame nearby. If something goes wrong,
hot burning acetone is hard to extinguish. I'd go electric, and I'd be more comfortable with a metal or a pyrex boiling flask.
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blogfast25
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| Quote: Originally posted by zed | | That appears to be a gas stove. Distilling acetone is no big deal, but I wouldn't fancy doing it with an open flame nearby. If something goes wrong,
hot burning acetone is hard to extinguish. I'd go electric, and I'd be more comfortable with a metal or a pyrex boiling flask.
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Yes, I would be more comfortable with electric heating and a metal or pyrex flask too. For now and for these small quantities it's a question of
keeping one's wits about, avoid leaks and keep the place well ventilated.
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Picric-A
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I have just bought 2.5l of L.G Acetone for £7, but having said that, when i needed to buy 'pure' acetone i would spend ~£1.50 for 50ml at a
pharmacy, as you did- thats almost $3 for 50ml, thats $150 for 2.5l ! :O
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blogfast25
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Where in England did you buy it?
Because I'll be using more acetone than originally anticipated (but still only about 50 ml per day for the zirconyl chloride project), I'll definitely
be drying/recycling/redistilling mine, possibly 'investing' in a few more bottles of no frills nail polish remover. Or make a few calls to local
businesses that may use it...
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Picric-A
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Blogfast25- check your U2U's!
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blogfast25
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Done! Thanks...
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blogfast25
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The still head has been modified and fitted with 2 brass pipes, more or less perpendicular to each other, connected in series to a gravimetric cold
water supply through silicone RC fuel lines. Photos, top: modified still head, bottom: still in operation.
Through some sheer luck this seems to have the right cooling capacity: with water full on and head temperature (thermocouple just above cooling pipes)
at 57.1 C (using virgin NPR feed) no distillate came over, not even a drop, not even after 10 mins. But shutting off the water and distillate
immediately started coming over at the usual rate of about a drop per second. Turning the water back on the distillate stopped coming over. So with
water full open its refluxing at 100 %.
Using a clamp on the silicone tubing, the water flow was sufficiently restricted so that reflux took place (very visibly) and distillate came over as
well. A needle valve will now be fitted to the water supply to adjust it more easily.
300 ml of NPR were distilled this way with a remarkably stable head temperature of 57.2 C (with reflux) which towards the end dipped to 57.1 C. With a
recycled acetone a consistent 57.4 C was obtained.
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