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aga
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Cheers!
Any data is good for this exercise.
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forgottenpassword
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Methanol 64.7
Methyl acetate 57.0
Acetone 56.5
Methyl acetate / water 56.1
Methanol / acetone 55.7
Methanol / methyl acetate 53.8
Etc.
[Edited on 16-9-2014 by forgottenpassword]
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aga
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Many thanks forgottenpassword.
It would be great to bring all the BP data for everything into one place, so anyone could look up the possibilities
I'll try to get the 'toluene' (i.e. Upper) layer distilled tomorrow and see what that brings.
Probably Benzene, and Dragon Bile.
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Amos
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By any chance, do you have the name of the product you are distilling? I'd like to look into this a bit for myself.
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kt5000
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Thanks for posting this aga. I've looked at the paint thinner aisle also, and all I find are complex mixtures like you have there. I wouldn't know
where to start such a complex separation. I may give it a shot!
I was looking at a product called Strip-X, if memory serves.
[Edited on 17-9-2014 by kt5000]
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aga
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Me neither, hence the simple distillation.
> I may give it a shot!
That's the Spirit (pun intended)
This tin says UN 1A1/Y1.8/100/14/E/B-1026/IMV which i need to look up.
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aga
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Seems that the UN 1A1/Y1.8/100/14/E/B-1026/IMV marking is more about the Tin than it's contents.
UN = United.Nations.
1A1 = Tighthead.Steel.Drum.
Y = Packing.Group.II.6.Moderate.Hazard.
1.8 = Specific.Gravity.
100 = Kilopascal.Pressure.Rating.
source: www.myerscontainer.com/docs/POP-MCC-Section.pdf
The B-1026 seems to refer to 'Heptanes'
source: http://en.wikipedia.org/wiki/List_of_UN_numbers_1201_to_1300
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Little_Ghost_again
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I found and posted a table from wikipedia, but my account was deleted! I cant find it now. But will search some more.
Basicaly I think it said you could add some Hydroxide and get the methyl acetate to gice acetone and acetic acid it also gave all the azeotropes
likely
http://en.wikipedia.org/wiki/Azeotrope_%28data%29
there you go that should help
[Edited on 17-9-2014 by Little_Ghost_again]
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aga
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Perfect LG2.
Thanks.
Sorry to unionised for not spotting the link at the bottom of the page in his earlier suggestion.
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MrHomeScientist
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That's very strange. Even all the threads you started have been completely removed, which is a damn shame because there was lots of good information
in those. U2U Polverone or woelen and find out what happened.
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Little_Ghost_again
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Quote: Originally posted by MrHomeScientist  |
That's very strange. Even all the threads you started have been completely removed, which is a damn shame because there was lots of good information
in those. U2U Polverone or woelen and find out what happened. |
It appears the quality of my writing was deemed spam by the protection software lol.
So I was DELETED!!!
No ones fault except maybe mine, I have asked for details via U2U of how to avoid this in the future. Yes a shame so much good information is gone
but..........
Fresh start and hopefully I can avoid spamming  . The irony of it is I posted
the wikipedia link above and it was just after that I was zapped lol.
Having seen the vast quantity of spam that has apered today after the protection was disabled, it is far better I understand how to avoid the
protection than it is to keep it switched off.
It is not fair on the Moderator and Admin team to have to waste so much time dealing with the huge amount of nonsense spam. So much time energy and
money is spent chasing people for downloading films etc, and yet spamming is allowed to clog the internet and ruin peoples enjoyment and experience of
a truly great resource such as the internet. I strongly believe that there should be severe penalties imposed on those that operate and use these
bot's (intentionally).
Maybe another option is for the software to place all spam (as it see's it) into another forum, and rather than delete accounts it places a ban upon
the names etc. At least then there is a chance for resurrection when the odd inevitable mistake is made.
LG
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aga
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Really ?!?
I'm doomed 
Today i started distilling the Upper layer, and stopped after 20 minutes because the VT stuck at 63 C all the way through.
Stuffing all the Wiki azeotrope BP data into a spreadsheet, the candidates for a BP of 63 +/- 1 C are :-
chloroform
n-propyl bromide + ethanol
ethyl acetate + methanol
toluene + methanol
n-octane + methanol
tetrachloroethylene + methanol
acetonitrile + methanol
isopropanol + methanol
n-hexane + isopropanol
n-hexane + tetrahydrofuran
cyclohexane + ethanol
cyclohexane + methyl ethyl ketone
As it is stated on the Tin that it is a mixture, forgottenpassword's suggestion that it is most likely an azeotrope, or complex mix of azeotropes fits
very well.
NTODN is also right, in that the 63 C fraction cannot be cholorform, as it ignites very easily.
The layer that floated on water appears to be a mix of toluene + methanol, seeing as they fit the BP, and are already stated to be in there.
Next is splitting the Toluene & Methanol ...
Surprisingly this mix might be split using water as an entrainer :
www.ijcps.org/issue7/p2.pdf
There is also is a 'polydimethylsiloxane' membrane which seems to separate out the methanol.
Haven't got one of those.
Making some CaCl2 instead.
[Edited on 17-9-2014 by aga]
[Edited on 17-9-2014 by aga]
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Praxichys
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Wash repeatedly in water.
Methanol is miscible with water in all proportions. Only half a gram of toluene will dissolve in a liter of water at 20C.
Shake your mixture vigorously with about the same volume of water, discard the water, and repeat 4 or 5 times. This will remove essentially all of the
methanol from the toluene. Shake the toluene over anhydrous CaCl2 to remove the last traces of methanol and water. Filter out the CaCl2 and distill.
You will then have reasonably dry and pure toluene.
You can obtain your toluene by using this same process on the 'Super Disolvente' directly, without distilling first, since AcOH, MeOAc, and acetone
are all very soluble in water, although you may have to perform the wash a few more times - perhaps 6 or 7.
[Edited on 17-9-2014 by Praxichys]
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aga
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Fantastic ! Thanks very much for that.
As the saying goes, Praxichys makes Perfect !
Edit:
Just HAD to go give that a try straight away.
Interesting result.
100ml 'Disolvente' in a 250ml sep funnel with 100ml DDIW.
Immediately two layers appeared.
On shaking vigorously, a milky white liquid occurs.
Left to stand for a few seconds, a slightly milky top layer formed fast, with the bottom layer less milky.
Draw off the bottom layer, add 100ml DDIW, shake, wait, draw off bottom layer.
Repeat 4 times.
At iteration 5, the Top layer became Clear, and the lower layer milky with tiny, but visible droplets.
Subsequent iterations yield the same, with the Top layer perfectly clear, which i took to be the point at which i could stop adding, shaking etc, as
the toluene is now as 'clean' as it can be with this water process.
Lesson learned : wait for advice from someone who actually has done this before and knows what to do !
[Edited on 17-9-2014 by aga]
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