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Author: Subject: micro distillation
Cheapskate
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micro distillation

Hopefully I'm going to have a small amount of a high boiling point liquid that I want to distill. Specifically nicotine. I have a separate thread over in bio that folks have been helping me with, and at some point, I hope to have a few ml to purify.

I know how to micro distill a few ml if I'm going for the lower boiling point fraction, but how does one get the higher bp fraction?

My 24/40 setup is just too darn large.
neutrino
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What you want is a book which talks about semimicro technique (dealing w/chemicals in the ~5mL area). Vogel’s 4<sup>th</sup> had a good section on this and I’m sure that the 5<sup>th</sup> (check the ‘FTP Server #2’ thread) is no worse.
sparkgap
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Mayo, IIRC, also offered pretty good advice on microscale techniques.

BTW, is this in the FTP?

sparky (^_^)

P.S. I am not too sure if microscale equipment can be had cheaply, though.

"What's UTFSE? I keep hearing about it, but I can't be arsed to search for the answer..."
flyingbanana
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Hickman still

try looking up Hickman still and setup for distilling a few ml amounts...
Cheapskate
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Actually, the hickman isn't the problem it's the fact that I need the higher boiling fraction. A hickman does a fine job of getting the lower temp fraction, but then you have to remove all the low temp stuff and then clean the collar and distill the rest.

It's tough enough getting the first batch out without losing it, but how do you get it away from the rest?
Eclectic
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[Edited on 4-3-2005 by Eclectic]
Cheapskate
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That setup is so cool. It's gotta cost U$1000 though. I'm gonna look in the catalogs to see. I'm sure I can't afford it. Eclectic International Hazard Posts: 899 Registered: 14-11-2004 Member Is Offline Mood: Obsessive Sometimes you can pick up something like that off of ebay for less than$100. Search for " short path" in glassware under buisiness and industrial. Or just see what turns up searching for 14/20.
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mick
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Actually, the hickman isn't the problem it's the fact that I need the higher boiling fraction. A hickman does a fine job of getting the lower temp fraction, but then you have to remove all the low temp stuff and then clean the collar and distill the rest.

If you are talking about small quantity at high boiling point, short path distillation might do. The kit is made out glass tubing. Blow 4,5 or 6 bulbs near to each other. The starting stuff goes in at one end and seal the end. Distil from one bulb to the next. When the first fraction distils warm the whole lot up and tranfer to the end, increase heat and distil the next fraction. By the time the stuff you want has been distilled into bulb 3 or 4 it should be OK. Use a glass cutter or something to separate the glass bulb.

mick
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What about the Micro Condenser and the Sublimation Apparatus made by UGT, they seem prety nice at first sight. Anyone experienced it of have some comment? BTW, i searched on Ebay for Micro and Short Path and nothing got out, i'll do it for 14/20 now.

 Sciencemadness Discussion Board » Fundamentals » Organic Chemistry » micro distillation Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues   » Detritus   » Test Forum