dada (Stranger)
05-10-02 16:16
No 307218
      bright star results on bezo/wacker unclear  Bookmark   

A foaf did the benzo wacker against my advice and when distilling the results he found that the temp on his thermometer were very strange since he had done it before and has always seen the temp go to 108 (in his case) breifly then to a favorable 133. This time he noticed the temp and color were strange. He finished the process anyway and tried the next step with his unknown product. Failure set him into a deep depression and he wondered what to do with the remaining product which has been hanging around in a freezer. It has the smell and flavour of real ketone but he is not very experienced in these matters. Can the sodium bisulfite be done on this to purify or does he need to try something else. Any info would be appreciated.
dada/formerly DeJay
 
 
 
 
    Antibody2
(Rehabilitated)
05-10-02 16:29
No 307222
      if your foaf followed BS instructions they ...  Bookmark   

if your foaf followed BS instructions they distilled the ketone, so there should be no need for further purification. but bisulfite is an excellent way of telling whether your ketone is ketone.smile

IMHO bisulfite is shitty way to try an purify the benzowacker, as benzoquinone has a double bonded oxygen too, i think it forms a bisulfite adduct as well as the ketone (could be wrong) but any of my foafs who triied purifiing post benzo rxns w/ bisulfite had headaches.

performic . . . .(sound of angels sighing)wink
 
 
 
 
    dada
(Stranger)
05-10-02 16:44
No 307230
      unclear  Bookmark   

thank you. My friend  has seen these discussed here. In reading the s/b thing he was thinking that if it wasn't all the proper ketone this would convert its wrong to right. When this suspect ketone was carried thru the al/hg step it seemed to do all the things it was supposed to but upon pulling the product from the rxn it just vanished. I mean it seemed to go into the washings.
 
 
 
 
    Antibody2
(Rehabilitated)
05-10-02 20:51
No 307297
      your foaf could take 1ml of this ketone and run a ...  Bookmark   

your foaf could take  1ml of this ketone and run a bisulfite test on it in a test tube, then he will know which step he fucked up
 
 
 
 
    Chromic
(Hive Addict)
05-10-02 22:00
No 307320
      definitely bisulfite it!  Bookmark   

Purchase some potassium metabisulfite, potassium sulfite, sodium sulfite or sodium metabisulfite from your local brew store. Dump 50g into about 100ml of distilled water, shake it up a few times, let settle (not all the bisulfite will dissolve)... then pour off about 5ml of the clear saturated solution of bisulfite into a test tube. Add about 100-200ÁL (0.1-0.2mL) of suspected ketone. Put a cork on, shake it up... let it sit for an hour or two. The whole test tube should fill with shards of bisulfite crystals if it's good ketone. If it goes sort of like chicken soup goo then there's ketone, but it's impure and needs to be distilled again.
 
 
 
 
    dada
(Stranger)
05-11-02 08:27
No 307412
      thats exactly what I needed to know  Bookmark   

Thanks Chromic, you are wonderful. I was getting lost in my reading. Have tried re-distilling before with no sucess at it. I think my set-up formed a leak and it all polomerized.(heat is a bad thing). Before, I relied on visual aids, and I read a post where someone wrapped his joints in teflon tape. When trying this I discovered that I actually lowered my boiling point(of not safrole) from 125c to 108c (obviously creating a better vacuum) I think I'll spring for a gauge this time and see just how good my aspirator really istongue Water pressure is terrific here and I use a low flow aspirator [$15]  Thanks again!

DeJay 
ps mr. moderator, is it possible to get my old username back?