ChemicalSolution (Hive Bee)
04-16-02 04:34
No 297482
      ideas for reducing et2O odor  Bookmark   

Is the procedure to make et2O from etOH in H2SO4 (@140) an unpleasent experience?  The main objective is to minimize the odor as much as possible.  What if she attached
a hose (connected to a water aspirator) to her vacuum adapter and turned the water on ever so slightly? 

How about during reflux?  The top of the reflux condenser is fit with a U-shaped adapter (packed with CaCl2 for water sensitive rxns) and set up like it would be for a downward distillation (so, using two condensers, one for reflux, one for un-coopertive vapors).  Would this contain the odor?


Or, Should she just run a hose from the vacuum adapter straight down the drain and turn the water on to flush it?

Run the hose into a water (alcohol?) trap?

Julia doesn't want to smell as much as a trace of ether (ok.. maybe a TRACE is fine :)

 
xoxo
Julia

 
 
 
 
    terbium
(Old P2P Cook)
04-16-02 05:00
No 297496
      Fortitude.  Bookmark   

That is real dedication when you even have to make your own solvents. Decades ago someone was telling me about working as a graduate student in a Soviet Block country and having to make many of their own reagents including even making their own benzene from acetylene.
 
 
 
 
    Rhodium
(Chief Bee)
04-16-02 05:11
No 297501
      ether vapor  Bookmark   

If faced with this task, I would use a liebig condenser as reflux condenser to cool the vapors, some kind of 180C connector and then a graham condenser with ice-cold water for downward distillation to trap all the diethyl ether vapors. The vacuum adapter at the bottom of the graham condenser before the collecting flask could then be connected to a tube leading to the bottom of a bucket of moist activated charcoal to trap any escaping ether fumes.
 
 
 
 
    Chromic
(Hive Addict)
04-16-02 05:19
No 297507
      Et2O  Bookmark   

is the procedure to make et2O from etOH in H2SO4 (@140) an unpleasent experience?

No. Be very careful, but it's quite easy. I do recommend that you have a pressure equalized addition funnel and a vigreux column with an efficient condenser. Make sure to use an oil bath, and run ice-cold water through the condenser. (alternatively, keep the receiving flask in an icebath)

The main objective is to minimize the odor as much as possible. What if she attached a hose (connected to a water aspirator) to her vacuum adapter and turned the water on ever so slightly? How about during reflux?

There is almost no odor when this synth is done correctly.

Or, Should she just run a hose from the vacuum adapter straight down the drain and turn the water on to flush it?

Not necessary, lead the fumes away from anything that could spark.

>Julia doesn't want to smell as much as a trace of ether (ok.. maybe a TRACE is fine

Why are you doing this procedure. It takes a hell of a lot of energy and time to make your solvents, I recommend you just buy the ether (starting fluid?) unless you're making this ether to huff. In which case, I hope you started from sugar, yeast, and good quality drain cleaner. Enjoy!

Don't break your glassware while huffing this stuff. (doh!) A vacuum adapter and a small flask make an awesome way to inhale the vapours, ensure that you wash it with sodium carbonate or it might taste a bit sour.. (ethyl hydrogen sulfate, yuck!)
 
 
 
 
    ChemicalSolution
(Hive Bee)
04-16-02 06:35
No 297539
      et2O  Bookmark   

She figues she can make it cheaper than she can get it from starter fluid..

Would you say she's crazy if she said she dreams of making ether, drying over CaCl2 and then distilling over Na for a Grignard!?!?!?

"If it can't be done OTC, then Julia won't do it." is what she says.

Rh--  SWIM know's that Mr Wizard has a massive Allihn condenser..  Maybe she'll sleep with him so she can use it... (j/k!)..  This would work better than a Liebig, no?


hugs and kisses- you guys..

Julia
 
 
 
 
    ChemicalSolution
(Hive Bee)
04-16-02 06:48
No 297550
      et2O purification  Bookmark   

In Vogel's book he gives a procedure for drying ether with Na wire.. There's only one problem.. He never says HOW MUCH ether can be dried with his "10g Na."

Any detailed write-ups on drying ether with Na metal? 
 
 
 
 
    lugh
(Moderator)
04-16-02 10:51
No 297643
      Science Writers  Bookmark   

Suggest you find a copy of the third edition of Vogel's; it clearly states that you use 7 g of Na for 1 L of ether smile It's doubtful that you will find any better written procedures than those in Vogel's, even around here laugh As far as dehydrating Et2O with NaOH (more OTC than Nasmile) see Post 247216 (lugh: "Re: Drying Ether With NaOH", Chemistry Discourse), the reference is in Post 247093 (lugh: "Re: Drying Ether With NaOH", Chemistry Discourse) smile