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Author Topic: Distilling mixtures that contain IPA  (Read 60 times)

reDEEMed

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Distilling mixtures that contain IPA
« on: July 21, 2011, 02:54:19 AM »
I used 91% IPA today as an experiment to see if it would extract a substance I wanted from a mixture of particulate. This particulate was not filterable as is and some sort of solvent extraction was absolutely necessary. As some of you know I'm only just now getting to play with all my goodies, a week now and I've barely slept  ;)

Ive been doing a lot of distillations and they are still new to me and I'm really learning as I go. The plan was simple, shake my water particulate mix with some IPA then vacuum filter and wash the gunk in the filter with some fresh IPA. Then distill of the alcohol to get back to my original amount of water plus substance and pick back up where I fucked up.

Well, this shit has been distilling ALL day. I've got way much liquid out of this than alcohol I put in, yet the stream has been steady. It's still holding the same temperature it was when the first few drops came over. Is it possible that all I'm doing is distilling water and the alcohol has formed some azetrope? Because I already emptied one flask with about 300ml in it that smelled strongly of alcohol, but I only put in 200ml of alcohol.

I'm writing off my substance as gone as of now, but I will keep playing with it to see what I can manage. But, what's the deal with distilling IPA?
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

reDEEMed

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Re: Distilling mixtures that contain IPA
« Reply #1 on: July 21, 2011, 03:06:26 AM »
Finally stopped. Temp jumped up and I shut it down. It still looks like more than I put in. It must be the few splashes I washed the filter cake and sep funnel with. Anyway, what's left in the flask doesn't smell of toluene or IPA, but it does smell like my substance. Who knows, maybe I did something right!

My luck is fucking uncanny. You can count on anytime I post a question on a forum, I'll have my answer in ten minutes. It just works that way for me, I dunno why.

I'd still like to some experience stories about distilling different things since I have plans to distill a bunch of different stuff to purify them, you know, hardware store solvents and such.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

akcom

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Re: Distilling mixtures that contain IPA
« Reply #2 on: July 21, 2011, 03:34:30 AM »
the azeotrope database is easily available (google azeotrope database)
http://eweb.chemeng.ed.ac.uk/chemeng/azeotrope_bank.html

isopropanol forms an azeotrope that is "87.9% by weight isopropyl alcohol and 12.1% by weight water" (wikipedia: isopropanol).  So yes, you distilled an azeotropic mixture of isopropanol and water

As the saying goes: UTFSE

edit: next time please give us the temperature on your still head

reDEEMed

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Re: Distilling mixtures that contain IPA
« Reply #3 on: July 21, 2011, 03:53:55 AM »
84C

I had no idea that azetropes where constant that way. I thought they were dependent on environmental variables, guess not. Makes sense now.

I really didn't know what to search for. I knew I started with an azetropic mixture (91% IPA, as always has some water) and I knew I would also distill an azetropic mixture, it just seemed like it picked up a lot of water from the boiling flask, more than it started with.

I didn't really know that azetropes were so predictable, sorry.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

akcom

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Re: Distilling mixtures that contain IPA
« Reply #4 on: July 21, 2011, 04:40:07 AM »

reDEEMed

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Re: Distilling mixtures that contain IPA
« Reply #5 on: July 21, 2011, 06:01:21 AM »
I have that book, the hard copy too. I took it out about an hour ago so I could start reading it again. When I read through it before I could not do any experimentation, so not much stuck. Now, I'm neck deep in in-process reactions, extractions, distillations and a buying frenzy of odds and ends.

I'll learn as I actually do things. Hopefully with time you guys will see that I'm not here so somebody will teach me to make some drug, I'm here to learn chemistry from people who actually do the kind of chemistry most relevant to my interests. I would put my money on one of you above some tightwad at a major chem joint any day. In spite of all their paper from this school or that one, I'm willing to bet they lack the macgyver type skill set that a clandestine chemist has to have. I'm a machinist by trade, I'm familiar with things like improvisation and precision. I admire these qualities in others as well.

I'm here to learn. Please be patient with me. Thanks for the advice, keep it comin'.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

reDEEMed

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Re: Distilling mixtures that contain IPA
« Reply #6 on: July 21, 2011, 06:58:54 AM »
HAHA, just got home, and in the spirit of digging out these books I bought, instead of the glassware, I grabbed my Merck. I'm ashamed to say I've not touched it since I moved. In my defense it was still packed and kinda outta sight outta mind. Anyway, just now is the first time I've really looked at it and holy shit! What a nice book. I like this book almost as much as some of my glass. I'm glad I never read or looked at it back before I moved, I think the anticipation would have killed me lol.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna
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