Author Topic: Christmas gear??  (Read 2886 times)

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  • Guest
Christmas gear??
« on: January 19, 2004, 11:53:00 AM »
Well, SWIRT has UTFSE until his hands are as numb as his brain, and he can't find any good answers to this:
Final product (rxn parameters to follow) melts to green, recrystallizes on foil to pink/red.

2gPfed/1.6gMBRP/2.4gI from tincture were combined in a 50ml Erlenmeyer flask, 1ml dH20 added before adding I2.  Normal reaction seemed to occur at ~100 C.  Cooked for 2.5 hours, everything seemed fine. (before SWIRT gets roasted for this, he was in a hurry and wanted something for the wife to be UP while he was LWRing)

Workup was as follows:
Filtered using charmin plug
Washed 3x, with cool, warm, really warm naptha
Based with 20% RDL/dH20
3x water volume of naptha was added, then washed (30min sit time) 2x with dH20
Gassed with Al/HCl dried over CaCl2
Snowy snowy snowy, just like Christmas
washed with acetone, recrystallized 2x via dual solvent
Beautiful crystals...that melt to green and crystallize to red/pink.
WTF is this?
Bioassay says twweeeeeekkkkkyyy shit.
Is this a contaminant from using RDL rather than NaOH lg?


  • Guest
Tweeky dope
« Reply #1 on: January 19, 2004, 02:21:00 PM »
In another thread Placebo and Geezmeister discuss the causes of tweeky dope

Post 482566

(placebo: "Geez, Re: I noticed long ago there was direct...", Stimulants)

How clean were your precursors?

Final product (rxn parameters to follow) melts to green, recrystallizes on foil to pink/red.

The green is most likely anti-histamine, CM.  The pink red indicates some sort of gakk and or excess iodine.

Washed 3x, with cool, warm, really warm naptha

Naptha is only effective when warm, near it's boiling point, as a post-rxn fluid cleaner.
Xylene and tolly make for excellent post-rxn fluid washes. In swims case his honey(post-rxn fluid) was always washed 3x with Xylene and 3x with the same solvent one is extracting with to ensure no trash. 
Read this for proper post-rxn method.

Post 428962

(Osmium: "RP/I2 post-reaction workup: The short version", Stimulants) :)


  • Guest
clean in=clean out, right?
« Reply #2 on: January 19, 2004, 02:37:00 PM »
Pseudo was cleaned via Tetra trap, washed 2x with cold water and recrystallized. The crystals were then dissolved in hot naptha and gassed to precipitate PseudoHCl. The pills, AL*****D contain no antihistamine that he can see actually on the package.  The I2 is exactly the same batch that he has been using, and the MBRP is fresh, today, er last night, or yesterday? Anyway, never run in a rxn.
This is about the 50th reaction for SWIRT and he has never seen this before.


  • Guest
You know, I could drop a few tiny, barely...
« Reply #3 on: January 19, 2004, 02:45:00 PM »
You know, I could drop a few tiny, barely visible crystals of methylene blue into your bathtup and you might wonder if I had filled it up with ink. Which proves that the right kind of "impurity" in ppm amounts (e.g. a strong dye) can impart a fucking intense colour to otherwise clean stuff (the water in your bathtub).

So you got some poorly cooked garage dope and it discolours when you heat it. Wow. Nerve-wrecking! Scary! Imagine this, if you heat it up even more it might turn black! Damn.


  • Guest
« Reply #4 on: January 19, 2004, 02:57:00 PM »
So where exactly would this dye impurity originate Os? If clean precursors were used, or as clean as can be made by klandichem methods, did SWIRT just get screwed somewhere by an inadvertant additive?
All glassware was cleaned beforehand via standard methods. (washing soda/dH20 rinse x3)
Impart some wisdom on SWIRT,Os, so he can at least know in which area to look.
Oh, and the pseudo burns pure, no black on foil, very VERY slight foil discoloration


  • Guest
"Burning clean" is no certified analysis
« Reply #5 on: January 19, 2004, 03:31:00 PM »
All reactions create byproducts. Without acid/base extraction of the post-reaction mixture, distillation of the freebase and slow recrystallization of the final hydrochloride salt, you will always have enough impurities in your product to make it possible that they could impart such a color upon heating of the salt.

See this report for example:


  • Guest
Anti-Histamine unlikely
« Reply #6 on: January 19, 2004, 04:41:00 PM »
Anti-Histamine unlikely if cleaned with tetratrap
Look more into the removal of OrangeII gaak
and cook longer.


  • Guest
skipped distillation
« Reply #7 on: January 19, 2004, 04:46:00 PM »
Thanks for the input.
It seems that SWIRT needs to do a distillation to avoid this in the future.  All the other steps were followed,ie A/B, slow recrystallization (2x) so this must be the problem.  It seems odd that in all the previous reactions, nothing of this sort was noted, even slightly.  Also the color change from melted to crystallized being so different on the spectrum puzzles SWIRT.
Alas, formal chemistry was far far in SWIRT's past, so many things puzzle him.


  • Guest
ghetto glass?
« Reply #8 on: January 19, 2004, 05:24:00 PM »
well, it sure sounds like you did the washes, and a rxn that small likely needn't reflux 'till next tuesday, and you had prior successes.

swimmy had incident of bafling color once from silicone caulk meeting ph 14 in a poorly crafted ghetto-sep funnel.

'tis true about color beeing imparted by contaminents that are in minute percentages.

how is it, anyway?

perhaps you synthed the messiah by accident.


  • Guest
re: christmas gear
« Reply #9 on: January 20, 2004, 12:34:00 AM »
if all you guys didn't smoke the stuff, it wouldn't be that big of a problem.


  • Guest
« Reply #10 on: January 20, 2004, 04:28:00 AM »
Blue or light green appearing when your gear is melted is most allways from traces of Tripolidine.


  • Guest
Ware is right
« Reply #11 on: January 20, 2004, 10:10:00 AM »
If swir used tetra, than it would have pulled any anti-hists out of the picture.

Aside from using a better NP to wash you honey withm, I see nothing that swir did wrong, besides the two hour cook time.  If that was as long as you had to cook should have use the push/pull.  It is most likely a tad underdone.
   Again take Ware's advice, he is right.
   Copper any where in your lab setup that the meth might make contact with will turn it green, Jacked had a post on this, UTFSE and you will find it.
    Go get some JD. :)