MR AZIDE - 23-7-2012 at 16:22
Bought a 400ml bottle of this stuff at a £1 a while ago, and had got around to distilling it the last few days.
I used some of the crude stuff for something else, but had 350 ml to distill.
Ingredients, were ( on label) and cannot find MSDS, Aqua, Acetone, Ethyl Acetate, ( some other stuff) glycerol, and a pink dye.
On using a quickfit distillation apparatus, the acetone fraction came over at about 60'C, and after distilling the whole 350 ml, stopping at before
the bp of ethyl acetate at about 77'C, , I had collected 200 ml of very nicely clear, mobile acetone, which had a smell of the ethyl acetate to it,
and it was confusing trying to distinguish between the two odours.
I was left with about 100 ml of the now more concentrated aqueous dye , the liquid turned red, and it became frothy to boil.. During distillation of
the last fraction, oily drops of what must have been the glycerol, which looked contaminated with something else ( brownish) could be seen bumping
about. There must only have been about 4 or 5 ml of it. The red liquid was non- flammable.
The 200 ml of distillate was redistilled, and the acetone came over at about 60 to 64'C, quite rapidly,, and i changed receiver flasks at about 175
ml of what seemed purer acetone........it smelled purer with no ethyl acetate smell detectable.
The next 50 or so ml in the distill flask turned milky, and a new fraction came over at about 78 to 85 'C, which smelled more like the ester , but
still smells quite acetone like, and was slower to drip into reciever, about 20 ml of this was collected.
the last 15 or so ml, was collected at about 85 to 98 'C, and was slower to collect. This fraction, smells almost entirely of the ethyl acetate
fruity odour.
The distillation flask contents were now very cloudy, and there was not much left in it. I stopped collecting at the 98'C, The liquor in the distill
flask remained cloudy when cold, and had barely any odour of anything. This milky stuff was non-flammable.
1)How was there still acetone present, in the fraction at 78 to 85, when this is quite a bit beyond the acetones bp of 56'C?, and the acetone should
have been all recovered.?
Also, how was there some ethyl acetate in the fraction at 60 to 64'C, when this is quite a bit below the bp of ethyl acetate..?
2)Do these two form azeotropes?, where a small bit of each is always going to distill over.?
3) is it typical for ethyl acetate ( or esters in general) to form milky emulsions with water when boiling down,?
The point of all this was an excuse to use the distillation stuff, of something bought OTC, with the enjoyment of the witnessing of distillation
process, and not so much as obtaining pure samples of each solvent.
You get quite a bit of satisfaction, watching this pink cocktail of stuff boiling, and then separating out and collecting these colourless,
components.
Redistilling the crude 200 ml was interesting as well.
I think I will be trying next the distillation of methylated spirit now, for a bit if fun, to see what I can get.
for a lot of you hardcore guys, who have been doing this for years this might seem mundane, but in basic hobby science, this was very interesting
for me.
[Edited on 24-7-2012 by MR AZIDE]
Lambda-Eyde - 23-7-2012 at 16:46
You haven't given us enough information to answer your questions. Did you use a column? What kind of column? Was it packed? What was it packed with?
What was your take-off rate, how long did the distillations take?
smaerd - 23-7-2012 at 17:13
4) Ethyl acetate is somewhat soluble in water, and if there is sufficient ethyl acetate it should form two transparent layers with water. Milkiness?
Not in my experience.
MR AZIDE - 23-7-2012 at 17:53
The condenser was a simple water cooled liebig, and was set up as a standard distillation, not as a fractional distillation, although re-arranging the
apparatus by connecting the condenser directly onto the RBF, with the still head , thermometer, and receiver adapter, connected to the top of the
condenser., an attempt at a fractional distillation could be tried.
The initial product, that was being distilled which turned deeper shades of red, due to the increasing concentration of the dye, also went milky as
well when hot,, but went transparent again when cooled.
The milkiness in the initially distilled 200ml crude acetone / ester mix may have been due to the other ingredients that were present in the product.
I think these other additives may have now been precipitated as a fine emulsion( insoluble in little water), since a lot of the organic components
of the product have been boiled out and collected, leaving only mostly the aqueous component.
Ive thrown out the original bottle mistakenly, and cant report on what these other additives are, unless I buy another bottle of the stuff......
[Edited on 24-7-2012 by MR AZIDE]