Author Topic: Seeking column and condenser opinions  (Read 99 times)

Greystalk

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Seeking column and condenser opinions
« on: October 26, 2012, 07:38:24 AM »
Seeking opinions on fractional columns and condensers to vacuum distill oil of sassafras albidum.
The lengths are all 250mm - 500mm.

Vacuum jacketed fractionating column:


Jacketed fractionating column with tip for vacuum:


Horizontal condenser for fractional distillation of safrole:




These vertical condensers are for reflux and hard to distill stuff.

Condenser for reflux (Al/Hg):


Allihn condenser for reflux (Al/Hg):


Coldfinger with coil for reflux (Al/Hg):



Distillation and reaction vessel will be a 2L - 3L 3-neck RBF.
Safrole distillation apparatus will have a RBF in an oil bath with magnetic stirrer and fractionating column connected via 3-way adapter to the condenser which drains to a 1L RBF via 2-way adapter.
The sourced Xylene and Nitromethane needs to be distilled too and there is hope that 3 pieces of condenser and column glassware will suffice for all of these.


I like the vacuum jacketed fractionating column (not the one with the tip for vacuum) and the coldfinger coil condenser for reflux.
Vacuum for safrole distillation will be applied at the 2-way adapter between the condenser and distillate RBF.

If you had to get only 3 pieces of glassware from those on top, which would it be?
Suggestions for a horizontal condenser for fractional distillation of safrole are welcome.

lugh

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Re: Seeking column and condenser opinions
« Reply #1 on: October 26, 2012, 05:18:49 PM »
You seem to be rather uninformed about what's been done to help people like you long ago elsewhere:

http://www.erowid.org/archive/rhodium/chemistry/safrole.distillation.html

http://www.erowid.org/archive/rhodium/chemistry/equipment/pictures/distillation_big.jpg

http://www.erowid.org/archive/rhodium/chemistry/equipment/distillation4dummies.html

and a link to Zubrick's here:

http://127.0.0.1/talk/index.php/topic,2443.msg24794.html#msg24794

instead of begging for spoon feeding  ::) The end results from the effort applied  8)

Chemistry is our Covalent Bond

Greystalk

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Re: Seeking column and condenser opinions
« Reply #2 on: October 27, 2012, 01:18:50 AM »
You seem to be rather uninformed about what's been done to help people like you long ago elsewhere:

http://www.erowid.org/archive/rhodium/chemistry/safrole.distillation.html

http://www.erowid.org/archive/rhodium/chemistry/equipment/pictures/distillation_big.jpg

http://www.erowid.org/archive/rhodium/chemistry/equipment/distillation4dummies.html

and a link to Zubrick's here:

http://127.0.0.1/talk/index.php/topic,2443.msg24794.html#msg24794

instead of begging for spoon feeding  ::) The end results from the effort applied  8)

Thanks for the kind words. Those links are quite familiar.

I'll rephrase, can one fractional distill compounds that have 5C - 25C between their boiling points with a Liebig and packing? I was assured this is was impossible, lab grade separation anyways without a Snyder column which isn't easily available to me.
It seems to work well enough as you are pointing me to Zubrick's and other setups with just a distillation head and no fractionating columns in some of those setups.

Distillation isn't new to me, but fractional distillation under vacuum is. Which is what brought about this thread.
Is it considered spoon-feeding to seek opinions on the glassware available to someone? Not everyone has access to a S-A catalog, or perhaps they don't want to go that route and are limited in options. This would not be an issue if one could just go back and keep buying glassware.

lugh

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Re: Seeking column and condenser opinions
« Reply #3 on: October 27, 2012, 01:45:15 AM »
Leibig condensers usually have nipples in them for retaining packing so they can serve double duty as distilling columns  ;) The procedure authored by Chromic on Rhodium's page explains exactly how to fractionate the essential oil from sassafras albidum, so perhaps one should try fractionally vacuum distilling some other organic chemicals first to gain experience since such essential oils are much more valuable now than they were at the time that web page was created  :-X  You can use a capillary tube for controlled aspiration instead of a magnetic stirrer if you're knowledgeable in their use  :P  As has been said before, the end results from the effort applied  8)
Chemistry is our Covalent Bond