05-17-02 10:09
No 309992
SWIM has already read all the thread he could find on ketone color but not able to get conclusive answer. Everyone seems to talk about antifreeze green and yellow ketone. SWIM is vac distilling ketone right now. It is clear and clear can be. SWIM vac distilled iso at 91C. This ketone has been coming over in the 104C range. Why would it be so clear. Using Oxone route.
Pardon my friend officer, He's a little slow.
(Stranger)
05-17-02 10:47
No 310008
If it is clean, it is really clear !!
You will only see a very light yellow hint if you have a good quantity of ketone in your flask.
You will be able to notice that it is more viscous than safrole, and that the smell is different. Smell is not very strong right out of the distillation setup, it is too cold. Put some on your finger and smell it !!!
(Greenhorn)
05-17-02 11:32
No 310024
When swim first ran the oxone method, his ketone was clear with yellow hints in it. Safrole distilled at 70-72c and ketone ~85c. Swim thought he fucked up and threw out the first run. It was about 25ml of ketone. After running it again and geting the same, swim ran a MM al/hg and low and behold lovely crystals. Swim was use to the antifreeze green color of benzo wackers and mistoke pure ketone for garbage.
We'll soon find out if I'm a chemist or not!
(Hive Bee)
05-17-02 11:55
No 310038
SWIM has taken of the vigreux column and is vac distilling some more. SWIM has kept the different portions seperate. Distilled iso at 91C. When distilling ketone got some clear stuff at and up to 100C. Dumped receiver and kept contents. Then started again with vigreux, this time caught the biggest portion around 103C. Dumped receiver and took out the vigruex. Now SWIM is seeing the green antifreeze shit. It is coming over at 120C, which is 29C higher than that of iso, which I assume is about 39-40C higher than that of safrole. So what is the issue? Should SWIM discard this highest fraction that actually has the green color or use it anyway. SWIM just wants things to go right that little color problems are very discouraging.
Pardon my friend officer, He's a little slow.
(Title on BackOrder)
05-17-02 13:19
No 310057
Swim had similar results once from a peracetic run. the first distillate sounds like unreacted isosafrole. The second run is probably your ketone, and the last run is probably glycol. try taking that last run and putting it in the freezer for a while. Does it become very viscous/syrupy, eventually freeze? if so, you probably did not reflux it in sulfuric long enough to hydrolyse it to ketone. If that is the case, run the hydrolysis step on it again to convert it to ketone.
did you extract your oil using DCM after the acid hydrolysis? if so, did you change your oil inbetween distillations? if not, you probably have DCM vapors in your pump oil, which will affect the pulling strength of your pump. that is why the isosafrole is coming over at 10C higher now. sounds like we run very similar pumps, as I usually pull iso over at 91C. if you have a small residual amount of DCM in your pump oil, your ketone will start coming over around 120C, and the last fraction is what you are looking for.
(I'm not Cheesie)
05-18-02 13:56
No 310462
The isosafrol will come over first, then any epoxide that was trapped will come over, then your ketone, then any glycol/diol that was left comes, and the glycol is green in color. Congrats!! Cheese is crying as his new mantle arrived yesterday and half way through ditilling 300gm of isosafrol, the receiving end of chees'es last and only condesor cracked and pop! luckily there was no vacuum on at time (ATM at 252°C) So the room smelled up nicely and cheese continued to finish up distillation by sticking the broken end of condensor into receiving flask. that will teach cheese for not using clamps to hold the condensor/flasks, stillheads in place. no wonder it cracked , all the heat and pressure it was under from previous distillations That's 2 condensors cracked in the same spot. time to invest in some clamps eh/ ? ARRG!
<Cheeseboy-a whiteboy with soul, like a black guy without soul
May De Sorce Bee Wit Chu-Always
(Chief Bee)
05-18-02 14:25
No 310474
To cite J.W. Zubrick - "Congratulations, You'll get the highest F in the class!"
(Hive Bee)
05-18-02 20:29
No 310579
Thanks goiterjoe and cheese:
Goiter: If you distill iso at 91C. What temps do you expect and collect ketone? What is the max temp you would pull ketone with your vac?
SWIM thinks you guys are right on the glycol. SWIM really had to crank up the hotplate to get the green shit to come over.
So the basic point of this thread is that it is okay and actually preferred to have clear ketone?
Pardon my friend officer, He's a little slow.
(Title on BackOrder)
05-19-02 08:30
No 310816
your ketone should look relatively clear with a yellow tint to it. if you're getting iso at ~90C, expect your ketone around ~110C.