Author Topic: waxy after a/b  (Read 1442 times)

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12cheman12

  • Guest
waxy after a/b
« on: June 20, 2004, 05:21:00 AM »
swim washed his pill mass in tetra then did an xylene soak.
He dried his pill mass and added equal parts sodium carbonate, activated with some metho and pulled with xylene.
After 2 pulls the xylene was added together and filtered clear.
Then titrated.
Once the water evaped there was some pin wheels... not the best but they were there.
There was also some kind of build up around some edges.
Anyways swim thought he was done, went to scrape up and instead of scraping up nicely it went kind of waxy.
He disolved this in metho then evaped but same problem.
He disoled back into water, filtered and added a NaOH solution till the freebase needles appeared then filtered (hoping the waxy substance will stay with the water this time).
Let the FB drain of all the water and hopefully taking the gunk. Took the freebase needles and coverd in some water and added dropwise of HCL and keept shaking till all disolved.
Then water was filtered again and set to evap.
The evap is about half way though, but the same problem looks to exist.
The pills are Aussie. 60mg pseudo 2.5 trip.
Anyone have any ideas.

p2e3r4f5e6c7t8

  • Guest
This has been answerd many times
« Reply #1 on: June 20, 2004, 05:47:00 AM »
So do some more reading and UTFSE :o


12cheman12

  • Guest
the best swim could find was looking through...
« Reply #2 on: June 20, 2004, 06:08:00 AM »
the best swim could find was looking through scottydogs thread.

"After filtering off the gassed pseudo and ditching the gakk ridden NP, he doesn't waste his time or precursor by rinsing with tone. He just scrapes the waxy pseudo "mix" from the filters into a clean mason jar, adds fresh NP, water and adds muriatic til it hits 6. Isolates the polar and evaps for pristine HCL."

I thought i did this already when i did the titrations, are you sayind i should just add extra HCL.

Shane_Warne

  • Guest
wrecked it at the end.
« Reply #3 on: June 20, 2004, 10:07:00 AM »
Once the water evaped there was some pin wheels... not the best but they were there.

Do you know what happened here?
pfed.hcl or pfed.h2so4 dissolved in the alcohol before your Na2CO3 dissolved, and migrated unbased to your xylene layer because alcohol and xylene are partially miscible.

Na2CO3 dissolves poorly in alcohol.

If your determined to use alky and/or acetone as a basing medium, in order to exclude H2O, in order to not activate certain gaks. Then it's probably best to follow the Waterless A/B how it's written...

you probably would have had better conversion if you heated the OH/base/pfed for a good hour or so, and then added the NP.


He disoled back into water, filtered and added a NaOH solution till

What did you filter out?
Because your OH basing probably converted some salt to freebase.


basing in OH has good potential to:

1. Give you a mixture of salt and freebase upon evaporation.
2. Give you a mixture of salt/freebase/extra gak upon evaporation.

3. Give you a mixture of sulfate and hcl salts if the NP is gassed or titrated with HCl, if the pills were sulfate.

4. Make it essential to rebase the lot.

5. Maintain a dry procedure  <-- at what cost? worth it?

Scottydog

  • Guest
Newer gakk has rendered this method obsolete?
« Reply #4 on: June 20, 2004, 01:59:00 PM »
"I thought i did this already when i did the titrations, are you sayind i should just add extra HCL."

Well first of all you pulled with xylene and went straight to titration. Which means any gakk that followed along with the pseudo into the xylene is now back in with your pseudo water after the titration with HCL.

The purpose of this method was to deal with the PH identity crisis that the gakks gave the resulting crude pseudo. Also to leave a majority of the gakks in the NP after filtering out the pseudo.

Then fresh NP is used (sans gakk) fresh water and the HCL drops the PH from 9-10 down to 6 where it belongs and sends it back down into the polar to bee isolated and evapped.

Im not quite sure if this method is still effective. Even newer gakks may have rendered this method obsolete like most of the other extraction techniques on this board.

Swim's last mishap included the use of a different NP (odorless MS) rather then Xylene.

Swim will revisit the modified tetra trap with gassing, going back to Xylene as the NP, with some precleaning of the GUPS first to see if this makes a difference.

Swim checked the lot #'s on the successful extractions and compared it to the failure and they were of the same lot.

The yellow oil started to release from the GUPS before any heat was actually used.

He usually mixes the GUPS and carbonate and sprays it down with tetra. Adds the Xylene and puts it on the coffee warmer. The water is added after the carafe is already sitting on the heat source.

On the failure using MS for the NP. The water had already been added prior to the addition of the NP and heat and the carafe had been sitting for 20 minutes before he finally got around to heating. He watched the yellow oil ooze from the tetra saturated GUPS! Maybee an excess of water was used, thereby releasing the gakks before the water had a chance to evap or get absorbed by the GUPS. All speculation of course.

The MS may have also had additional "entrained" water?

Swim will try a 24 hr gum spirits soak prior to the original extraction method.

Concerning overall yields, Swim is not that impressed with either the gakkinator or Fester's method.

After all of this time, money and solvents, Swim could have very easily afforded a semester with two classes of Org chem at the University, had basic distillation methods down to a science and been half way to a successful L-PAC biosynth by now.  :(  Eventually, these fuckers will bee getting rich off of someone "other then Swim's" failures.

Swim has been here too long to stay with pills and bee happy about it. They can find a new generation of suckers.  >:(  

Something to think about... and Swim is tired of JUST thinking about it, ya know?