06-12-04 01:47
No 512933
And we aint talking bowel movements btw..
So good old Swimmy McSwims-a-lot ran himself a small 2 gram reaction, all went well, and the resultant rxn fluid was steam distilled etc.. Titratred, acetone flashed, what-have-you.. Yield looked pretty good judging from what went in..
He got some very nice looking bright white crystals/flakes.
Some was ingested, and found to be decent.
Burn test on foil revealed very little whitish residue.
All was splendid.. Until swim decided to recrystallize, at which point everything went motherfucking pear shaped.
He dissolved his shit in denatured alky, which was then heated to a boil. He noticed some fluffy looking shit forming in the alky as it was heating, and this was filtered out. He put the alky back on the heat to reduce it to saturation. As the alky approached saturation, it turned a redish color, and a sweet kinda marzepan smell was noted.
Not good. Swim evaporated a little of the alky in a glass dish, and the resultant product looked fine until it was scraped up, at which point it looked orange and was kinda gooey. He did a burn test on some foil, and the stuff bubbled and sizzled and turned bright red. Once it had vaporized, there was left a black looking residue on the foil.
"What the motherfucking fuck!?!", swim thought.
Now swim posts very rarely, choosing instead to UTFSE and usually finding answers to his questions. However he was unable to find anything really specific to this situation. Maybe it's due to the fact that the words he had to use for the search are quite common on this board. But anyway, he appologizes if this stuff has been dealt with before.
Also swim would like to add that he used red-hots as a source of p-fed, and used the KOH extraction method, which seemed to award him some fairly clean pseudo. He guesses it kinda looks like it may not have been so clean after all..
Anyway, if anyone could offer some advice on how to proceed, it would be greatly appreciated. Thanks!
(Hive Bee)
06-12-04 02:10
No 512934
swibbs seen something similar : Post 467029 (barkingburro: "ok... the shit's pink... HOT PINK", Stimulants)
my guess would be that the pink is a byproduct of an excess in phos. i have no empirical evidence but swibb knows that rp becomes h3po3 and eventually h3po4. now h3po4 is added to softdrinks for it's help in bubliness and for it's sweetness. and it seems like a posibilty. another possibility is that there is either a> residual NaOh or b> residual whatever NaOH + HCl makes (though i am pretty sure that makes NaCl and H2O). either way swibb's been able to get rid of it by rextalizing, just not in denatured. use 91% or higher IPA as NaOH has a low solubility in IPA. ANd so does NaCl. i think.
(Stranger)
06-12-04 02:21
No 512937
Hey man, thanks for the reply.
The one problem i have with your theory, is that when swim first evapped the water after titration, the stuff was fine.
It's only once it was dissolved in denatured alky and reduced to saturation that the red showed up.. COuld it be trash from the alky?
(Hive Bee)
06-12-04 03:09
No 512946
Was your beaker/container clean? Like REALLY clean?
(Stranger)
06-12-04 03:40
No 512949
The glassware was clean.. Not sure about REALLY clean.. But uh.. Well not sure how clean REALLY clean is.. Cleaned with water.. Maybe that's not enough? I dunno..
You know come to think of it, this has happened before.. But color was more orange than red.. Can't remember how it was dealt with , was a while ago..