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aga
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and i Thought i just bought some Toluene ...
At a big hardware store in Malaga i bought a 1L tin of 'Super Disolvente' which stated on the can :-
Toluene, Methanol, Methyl Acetate and Acetone (Propanone, Pah!) as ingredients.
I read that Toluene isn't soluble/miscible with water, so i dumped 500ml into some water and then into a separatory funnel.
Within a minute two distinct layers formed, so based on density, i assumed the top layer to be mostly Toluene.
Distilling the Bottom layer, i have seen 11 distinct B.P.s held for at least 2 minutes each, distillates of which which were separately collected and
stored, and have been trying to identify them by their BPs.
7 of them appear to be :-
56 - 59 C Methyl Acetate + Acetone
62 - 63 C Chloroform (!)
64 - 68 C Methanol
69 - 72 C Hexane
76 - 77 C Carbon tetrachloride
78 - 79 C Ethanol
80 - 83 C Benzene
I would appreciate some suggestion what the other 4 might be, as i can find no data for probable candidates :-
74-75 C
83 C
84-85 C
86 C
11 substances so far, before even starting on the larger Toluene layer !
All distillates ignite easily, and some smell very different to the others.
EDIOT : (an idiot editing)
80 - 85 C Benzene
changed to what the notes *actually* say : 80 - 83 C Benzene
[Edited on 16-9-2014 by aga]
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forgottenpassword
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If chloroform, carbon tetrachloride and benzene were present, they would surely be soluble in the toluene layer rather than the water layer.
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unionised
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God knows what you have got there but you need to be aware of this
http://en.wikipedia.org/wiki/Azeotrope
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aga
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Where the Toluene is will remain a mystery until i heat it up to 110 C
I just assumed it'd be in the top layer, but i could easily be 100% wrong.
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aga
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Azeotropes are probably in there in abundance !
Would you happen to have any link to a table of the BPs of some azeotropes?
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Amos
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Neither chloroform nor carbon tetrachloride can burn or be ignited. I also have to agree that those two and benzene would certainly dissolve in the
toluene rather than the aqueous layer(although you neglected to mention how much water you added, so that could complicate things. But if you still
want my input the 83 C distillate could be ispropanol. And there could also be a million different azeotropes happening here. Not to say that that
these separations can't be done with time and effort, but it's not nearly as simple as you're making it out to be.
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Amos
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And rather than try to identify them by their boiling points, start to examine the properties of each of your distillates (try salting some of them
out, for example, and see what happens)
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careysub
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One strategy to try with processing this 'witches brew' of solvents is to let CaCl2 soak up everything it can first, this should remove all alcohols
and acetone and simplify the distillations I would think.
I suppose with sufficient heating the alcohols+acetone would be distilled off the CaCl2?
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Amos
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How does CaCl2 get rid of the alcohols and acetone? Doesn't it only take in water?
[Edited on 9-16-2014 by No Tears Only Dreams Now]
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aga
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A quick google says that Chloroform does not burn per-se, but decomposes rapidly releasing, amongst other things, Hydrogen, which does.
Carbon tet seems not to burn at all.
I thought i'd start with BPs as i like distilling stuff, and can do that.
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aga
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I am sure it isn't, however i'm just telling what i did, and asking for advice.
There is no radical new theory being put forward here, it's just a noob with a disty rig and a bottle of Dissolve-it-All, wondering what is in it.
[Edited on 16-9-2014 by aga]
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careysub
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It is well know for taking up alcohols, forming complexes, but it does this to acetone also, though apparently not as strongly:
http://pubs.rsc.org/en/Content/ArticleLanding/1917/CT/ct9171...
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Dr.Bob
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I would guess that the 76-77 range material might be ethyl acetate, it is common in paint thinners and such, and might be somewhat water soluble.
I agree that 2-propanol would be around 82-83, that would be somewhat water soluble as well.
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aga
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The Assumption is that the Lower layer, which was distilled, is the non-toluene layer.
I don't know anything at all about it really, just that it was the Lower layer when about 15~20% by volume water was added.
The Upper layer was visibly more viscous, reacting in a 'lazy' way when the flask was tapped.
The Upper layer also burns easily, with an orange flame, and lots and lots of soot. Almost like a burning rubber tyre.
The Lower layer distillates all burn with a blue, or barely visible flame, and no soot at all.
Some have an orange flame, but still no soot.
All are easily ignited.
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forgottenpassword
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It doesn't contain ethyl acetate. The 'fractions' comprise a continous range from 53 to 86 Celsius -- supposedly WATER-SOLUBLE hexane, benzene,
chloroform and tetrachloromethane! It is a nonsense.
I would say that it is a fair bet that the stated ingredients are far more accurate than this attempted fractionation. The flammable distillates are
obviously various ratios of methanol, methyl acetate, water and acetone.
[Edited on 16-9-2014 by forgottenpassword]
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kmno4
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Quote: Originally posted by aga  |
(...)
7 of them appear to be :-
56 - 59 C Methyl Acetate + Acetone
62 - 63 C Chloroform (!)
64 - 68 C Methanol
69 - 72 C Hexane
76 - 77 C Carbon tetrachloride
78 - 79 C Ethanol
80 - 83 C Benzene
I would appreciate some suggestion what the other 4 might be, as i can find no data for probable candidates :-
74-75 C
83 C
84-85 C
86 C
11 substances so far, before even starting on the larger Toluene layer !
(...)
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Another spammer's crappy post......
With your total lack of chemical knowlede, you will harm yourself, sooner or later.
Better start collecting stamps, not impossible to get fractions.
Grow up and post no more.
Слава Україні !
Героям слава !
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aga
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As i have said at least twice, i could easily have the Water solubility entirely wrong, both in Identification and most likely in Concept.
Varying ratios of 4 ingredients leading to 11 multi-minute Stable distillate vapour temperatures ?
Fascinating.
Not having much understanding (or any stock) of Phase diagrams, i would be very appreciative of an explanation of how that can happen, if your
suggestion is that they form multiple azeotropes, and also somehow break azeotropic state to yield distillate, hence breaking the azeotropes they take
part in.
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aga
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| Quote: Originally posted by kmno4 |
Another spammer's crappy post......
With your total lack of chemical knowlede, you will harm yourself, sooner or later.
Better start collecting stamps, not impossible to get fractions.
Grow up and post no more. |
Thanks sooo much for the Honest feedback.
I wish my chemistry knowledge were as Comprehensive and Utterly Complete as yours, so that i could also Stamp on noobs with impunity, with the full
force of my thereby Fully Justified self-righteous pomposity.
Oh ! Crap. Appologies.
I posted this in the wrong forum - it should have been 'Beginnings'.
Thanks for pointing that out Clearly, and Succinctly.
(mod please move it to the right place. Detritus or Beginnings, you chose)
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Bert
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Thread Moved
16-9-2014 at 13:50 |
forgottenpassword
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| Quote: Originally posted by aga |
Varying ratios of 4 ingredients leading to 11 multi-minute Stable distillate vapour temperatures ?
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Yes, that seems most likely. The boiling points of your supposed fractions cover such a large and continuous temperature range that the idea of these
being discrete azetotropic mixtures seems unlikely.
[Edited on 16-9-2014 by forgottenpassword]
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Bert
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Moved as requested-
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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aga
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thank you Bert
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aga
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| Quote: Originally posted by forgottenpassword | | Yes, that seems most likely. The boiling points of your supposed fractions cover such a large and continuous temperature range that the idea of these
being discrete azetotropic mixtures seems unlikely. |
The thing is, each temperature range held for several minutes, some 5 mins+, which led me to think they were distinct compounds or mixtures.
Can complex azeotropes do that ?
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forgottenpassword
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Maybe they are azeotropes then. If you are certain that they are fractions then looking up data for all of the different possible azeotropes and pure
components will help you to identify the fractions, if that's what you want to do.
I see no reason to assume contamination from unlisted components -- especially those which would be poorly soluble in an aqueous layer, as previously
mentioned.
[Edited on 16-9-2014 by forgottenpassword]
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aga
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Would you happen to have any links to azeotrope BP tables handy ?
Not Certain at all, just saw the thermometer in the still head Hold at the stated temperatures for many minutes before rising, at which point i
switched receiver vessels.
[Edited on 16-9-2014 by aga]
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forgottenpassword
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Some are listed on the Wikipedia azetrope (data) page. I don't think that the relevant ternary azeotropes are included, though.
[Edited on 16-9-2014 by forgottenpassword]
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