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bees...analyze my nightmare
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| Author | Topic: HELP bees...analyze my nightmare |
| Chilly
Willy NewBee |
posted 02-05-2000 02:57 AM
Ok....I just woke up from this crazy dream. This guy was on his way with the BS method when he came to Step 3. Everything was follwed to the T, and going like clockwork until he flooded the reaction mix. Instead of two distinct liquid layers he got a 70/30 liquid, tomato-soup upper layer...and a pitch-black, crystal/goo layer on the bottom...to make it worse when the 2 liter bottle was shaken...to goo coated the inside of the plastic- making it even harder to distinguish the layers. The goo was eventually seperated...and was noted to have quite a bit of oil in it. The upper layer was washed with DCM...and everything seemed ok (clear orangish liquid came out). BUT- when the organic goo layer, DCM washes, and 150 ml 10% NaOH solution were added everything turned midnight black. NO chance of distinguishing layers. Light didnt even penetrate. He thought adding the last 150 ml of NaOH solution to everything might make the layers more distinguishable. It didnt...and now hes left with a mix of 300ml 10% NaOH, 200 ml DCM washes..and probably 100-200 ml of black organic layer mixed in. Please tell him this mixture can be salvaged...it took so much work..and the wanna-bee's hands are stained brown with that damn wacker mix. How can his hands be cleaned- BTW?? Anyway- the mix was chilling in the fridge...when I woke up...what can be done with this. I tried the search engines about this dream...but there are so many different variations of the wacker- he really needs something specific to this situation. If the goo layer is hydroquinone, why so much?? Do I have to chauk this one off as a nightmare?? Is this how the bs dream usually goes?? If not...how do I prevent future nightmares?? ------------------ |
| Icepick Hive Bee |
posted 02-05-2000 03:24 AM
Plastic sep funnel? yuck....things dont stick to glass as much....anyhow on to solving your problem. Vac filter the mess that should remove a lot of your free floating quinone, in the future if you have all those gold n black xtals in your dcm washes before you add the 10% NaOH you should filter there first, and that will clear up most problems in seeing the layers. They dont make a light strong enough to see thru the layers, you hafta shine it on the front/side and look for that green/black sep line. If worst comes to worst you can put everything back in the sep funnel and drain until you have 300ml left in the sep funnel, since this is how much 10% NaOH ya added is...its ok if you get some of the NaOH/quinone in the dcm stuff, itll distill out in the next step, just a small extra fraction that may add a little time, but wont mess anything up. Remember the point of this fractional distillation is to get the compound ya want (ketone) out of the post wacker tar crap, so you just discard anything that comes over that isnt in the temp range you are expecting. You havent fubared it yet, this is normal, keep going, youll make it 
Icepick |
| Chilly
Willy NewBee |
posted 02-05-2000 04:19 AM
Icepick..thx for the quick response. I just remembered some distinct details from the dream. First of all...there was a sep. funnel...in the dream...but it was only 500ml. It was kind of difficult for him at the time to seperate the black goo from the 1.5L aqueous HCL layer with a 500mL, narrow-stem (potential clogging) sep funnel..so...what he did was just take the 2-liter...and pour it through a coffee filter. Took all that goo/oil out like a champ. Anyway..the aqueous was now free from hydroquinone, and the organic/goo layer completely...so the dcm washes went like a snap. Clear orange liquid right?? So anyway..the problem is this..in the future how can the goo...be seperated from the organic layer??..or is the GOO the organic layer?? He was under the impression that the organic layer was just an oil. Also, there were alot of shimmering crystals when everything was first flooded..but it seemed like they dissolved as time went on. Anyway...his sep funnel is obviously too small to drain off the NaOH layer (unless everything was shaken up well...and done half at a time..would that be accurate enough??) or should he just continue with distilling. I was also wondering though if all that extra hydroquinone, and NaOh/Water might decompose the ketone faster, or make everything thicker..making everything harder to distill- (or bring the fractions closer together)...making it harder to distingush the ketone. This is a concern...because this guys safrole came over at 160 (very borderline vac)...would it make it that much harder to distill everything off with all the extra compounds?? In the future should this goo be vac filtered and pitched..or should it be thrown in with everything else...like he did this time?? One more thing...it was said in the writeup that the hydroquinone would clog the condensor..if he trys to distill...wont this happen?? Or will it be held in solution?? ------------------ |
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