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Author: Subject: Wheeeeeeee (kend)
aga
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[*] posted on 29-5-2016 at 14:27
Wheeeeeeee (kend)


New 'hood, new impetus to actually Do stuff, so here's what happened.

Started slow, and got more ethyl acetate from Nail Varnish Remover.

EtOAc.JPG - 82kB

600ml distilled, and quite a large volume of sweet/perfumy stuff separated and bottled (the ethyl acetate separately, of course).

Sticking any kind of funnel+valve (sep, peq etc) at the output of the condenser makes it really easy to 'cut fractions'.

Just turn the valve and collect/discard whatever fraction you like.

The new fume hood's extractor fan is garbage, so the 'hood cannot be used for Chlorine et al until the fan is upgraded (next week).

What next ?

Made stacks of sodium acetate quite a while ago just itching to become glacial acetic acid. Here's the last part of the 1kg batch :

crystalia.JPG - 110kB

Boil it up (after drying it) with conc sulphuric and make GAA !

rigged.JPG - 92kB

What next ? Erm, Volanschemia's winning entry in j_sum1's 'Lab from five OTC items' competition
http://www.sciencemadness.org/talk/viewthread.php?tid=64317&...
is Totally Inspiring, so i got some Xylenes then, well, you know ...

Graham.JPG - 75kB

First time that Graham condenser has seen any action (i didn't know what it was supposed to be used for)

Xylene.JPG - 107kB

The pot permanganate certainly leaves a stain ! (especially when you spill a spatula-full into the water bath).

Pretty sure i messed the reaction up as it still reeked of xylenes after all the KMnO4 was added.

Plenty more of both, so some experiments to try there (e.g. add the pot. perm. in Solution, which sounds more sane at the mo).

Something must have happened, because after filtering, then adding conc sulphuric, a white precipitate did indeed 'crash' out.

It happens immediately as each drop of acid is added.

Precip.JPG - 92kB

All-in-all, not a lot of Science done, yet a whole pile of thoroughly enjoyable Chemistry !

Wheeeee !

[Edited on 29-5-2016 by aga]




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Mood: Ever so slowly crystallizing...

[*] posted on 29-5-2016 at 15:34


That's a neat idea, using an addition funnel as a fraction collector. Now I wonder how well mine would hold up to vacuum...
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aga
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[*] posted on 30-5-2016 at 14:03


Is there any actual reason why the KMnO4 must be added as a Solid into a watery solution ?

It seems silly.

There is a utoob vid where some really unusual glassware is used (UC235 ?) to corkscrew the powder into the pot.

The same video mentions the possibility of over-oxidation, which is probably what i ended up with, being impetuous.

Why not just dissolve the pot permanganate and dribble it into the reaction vessel ?

It'll drop into water anyway, so what would be the difference, especially as the Xylenes don't mix with water ?

Edit:

Yeah, it was UC235 : https://www.youtube.com/watch?v=PAARYmBYudg

[Edited on 30-5-2016 by aga]




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[*] posted on 30-5-2016 at 14:36


Quote: Originally posted by aga  

Why not just dissolve the pot permanganate and dribble it into the reaction vessel ?



The reaction between KMnO4 solution and xylene is likely to be quite slow, compared to using powdered KMnO4 (think collision theory).

How do you plan on separating the various isomers obtained?

[Edited on 30-5-2016 by blogfast25]




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