Amicus (Newbee)
05-14-02 01:51
No 308175
      What am i forgeting?  Bookmark   

Ok I have...(doing KOH isomerization, oxone,nitro, hcl gassing)

Hermetic refridge compressor
24/40 vacuum distillation kit, 1000 ml capacity, 200mm vigreux, 200ml liebig
stirrer
a shit load of thermommeters (I cant tell you distillation virgins how bad it sucks to have ONE thermometer and break it! And have NO chem shops in your side of the state)
hotplate/stir combo
2000 ml sep funnel
stands, clamps
egg stir bars 32mm x 16 , that will fit 1000 rbf and stir properly correct?
digital scale accurate to .1 g
That should be all the hardware huh?
save for some coffee filters and plastic funnels, and some pyrex to do misc. mixing pouring in ect..i do have one 1L erlynmeyer for previous fun. Ill need some hoses for the vaccum hook ups and condensor....

What am i missing????

Thanks guys


"Not one shred of evidence supports the notion that life is serious"
 
 
 
 
    metwurst
(Newbee)
05-14-02 05:12
No 308207
      Vacuum trap  Bookmark   

If you're using a fridge compressor, you'll need a vacuum trap. Fridge compressors tend to be much less resilient to attack by solvents and acidic vapour. Let me assure you that your vacuum pump dying two hours before you've finished distilling your carefully prepared ketone will cause you immense grief and regret. Not as much as running over the cat whilst backing the car out, but it's up there on the list of things most likely to ruin your day.

I also see no mention of a thick walled filter flask, or buchner funnel. Given you have the vacuum pump, and a funnel/filter set is not expensive, you'll thank youself for getting one when you need to filter the KOH after isomerization. Also, they're just plain useful to have around.
 
 
 
 
    Chromic
(Hive Addict)
05-14-02 06:26
No 308229
      Filtering  Bookmark   

There is no filtering after the KOH isomerization. Distill it straight from the flask, do not use CaO.
 
 
 
 
    Amicus
(Newbee)
05-14-02 08:34
No 308265
      yeah  Bookmark   

I thought about a Buchner but they are expensive and none of the used ones i find have the rubber sealer, they are all so small too. I dunno i SHOULD have one though, your right. As far as KOH, i distill the iso right out of the flask, plus some oil in the flask to keep form crudifying the thing with koh flakes.

"Not one shred of evidence supports the notion that life is serious"
 
 
 
 
    metwurst
(Newbee)
05-14-02 10:10
No 308300
      Ah, of course.  Bookmark   

metwurst had been filtering the KOH out afterwards (and not using CaO) because he thought leaving KOH in might lead to slightly less byproduct being formed. metwurst initially began with the CaO at atmospheric, but was more satisfied with the vacuum reflux.

Then again, if 14 hours of reflux at ~120C doesn't hurt it, another 4 hours at the same temperature for distillation isn't going to hurt it either.

Thanks Chromic, for joggling my brain.