New Straight to E -- a novel extraction tech.

[newworldorder]

... is that I cannot buy you a beer and express my heartfelt appreciation for your breakthrough, in person.

Because, HOLY FUCKING SHIT THIS WORKS.

You are the man.

[geezmeister]

Nasty stuff it is indeed. This appeared after the second naptha pull, when I went to xylene and let it set. Has the amine in its tight little grasp and ate the better part of my yield from the Zyrtec tabs.

This is the variety of Orange II I believe. I will know next time to carefully a/b the pseudo from these tabs. I will have another batch before long and will update the notes.

The significance here is that it came through this process with the pseudo.

[xboXer]

I read that last post 5 times and I STILL don't know if I understand what the hell it is saying. Just a little about cops forcing an inactive addition while keeping the additive from the inactives list? Am I close?

[Sandman]

Just a note for those using Tyvek as filters: Tyvek is made of spun HDPE. The Chem Resistance Chart in VWR's catalog shows MEK or Acetone may do immediate damage at 20 Deg C. Don't know if that means it melts, decomposes or what, so you may want to be careful with your Tyvek and those solvents when heated or in full strength.

[Sandman]

It wasn't mentioned, but for NewBees, MEK can hold as much as 12.5% H2O @ 25 deg., so if you think you see some of your shiny new crystals vanish in final MEK rinse, they probably did!

Easy to fix. First dump just enough MgSO4 (epsom salt) to cover the bottom of the first beaker (after removing the already used drying agents), and fill with the amount of MEK you want for the final wash so it can dry out while you're recovering the crystals you just lost.

Now pour solvent with the wet MEK that melted your crystals back into the last beaker used, and evap until DRY (don't rush and burn product). Reheat residue with fresh dryed naptha/xylene (estimate amount from lost crystal wieght), filter as before, but this time finish with your now DRY MEK by pouring it - through a filter - directly over your recovered crystals.  Next time remember to dry your MEK first, just like the other solvents used. Note: Acetone can be even wetter then MEK!

[ChemNewbie]

Tyvek is made of spun HDPE. The Chem Resistance Chart in VWR's catalog shows MEK or Acetone may do immediate damage at 20 Deg C. Don't know if that means it melts, decomposes or what, so you may want to be careful with your Tyvek and those solvents when heated or in full strength.

Thanks for the heads up. I checked my VWR and it does indeed have acetone/HDPE listed with NN. That's really weird, cuz I've had gallons of dry acetone stored in Nalgene HDPE bottles, some of them for over a year, and the acetone hasn't so much as discolored the plastic. I checked some other compatibility charts, and some of those had HDPE listed as having excellent resistance to acetone. One military chart even had HDPE ranked right up there with FEP teflon. I wonder why? I rarely use MEK, so I'm not really worried about that.

CN

[mickyfinn]

I read that last post 5 times and I STILL don't know if I understand what the hell it is saying. Just a little about cops forcing an inactive addition while keeping the additive from the inactives list? Am I close?

SWIM thinks he needs a clarification for which post you mean... ...and what other vehicle the problem children could/might use to join the party other than the psuedo...granted SWIM can be a rather dense forest at times.

SWIM ran a tyvek trial and it was not the rounding success he envisioned. Now clearly, SWIM has a penchant for multitasking and the facilities just aren't set up to support it so much as retard it. From what he told me thogh the boatload of product either never made the journey out of the wrap or it was burned up in a ring at the bottom of a 2L filter flask when bringing the temp to 105. Zero fred appeared from 8 boxes of 24....then he lost his mind and forgot to crack the 120 name brand bluestamps in an attempt to salvage something from the night. Sure was fun straining out that plastic...after the damage was done.

So SWIM is going to see if an alky soak/pull in tyvek will produce fred.

In the meantime, last night he was able to run the STE using eight blisters of 24 each white 60's..."bullseye" brand that ryhmes with market...he is not thrilled with the fact that the fred pulled and then rinsed with plenty of MEK proceeded to turn orange when heated on foil...while the last perigogo's did not at this stage.

SWIM is gaining a little more insight each time as to the nature of the process of fred via OTC and hopes to one day contribute something of value to the bees (before he concentrates on any method besides pill extraction) for the assistance he has been given here in the forums to dream his own dream...

Now, however, he's off to see about putting together the pieces of pipe for a ghetto distillation setup currently on the non-existent bench.

[Sandman]

Is there any reason %Yield can't be figured by simply subtracting it's wieght from the full wieght of original pills and comparing to wieght of dried solvent residue?  Wouldn't that give a better idea of purity (if residue is void of bitter pseudo taste)? Just a thought . . .

[chronic_cook]

Just an other STE extraction... FUCK SWIC remembered he didnt have anymore MEK.

With some acetone at hand, SWIC dryed the extractions and it certainly had some other crap in it. It then boiled in 200ml xylene on high heat for a few minutes & decanted (~85% of it) then crashed w/ nice cold dry acetone.. SWIC discarded a gram or two of dirty goods. But finally SWIC got around a 70% yield. They were sparkly, salt-like pseudo crystals.  very clean!!

[geezmeister]

Translation, since even with the gakk the effect was felt from what was extracted:

Geez Gakked by zyrtec-D: Geezemeister's extraction of Zyrtec-D tablets by the Straight to E method alone resulted in the extraction of pseudoephedrine which was contaminated with the pill additive called Orange II by those bees who have written about it.

Nasty stuff it is indeed. Orange II gakk is not something you wish to deal with post-reaction as it destroys yield.

This appeared after the second naptha pull, when I went to xylene and let it set. The Orange II gakk only appeared in the third pull from the reaction fluid, which was done with xylene rather than hot naptha, and was allowed to sit in contact with reaction fluid overnight before being processed further. Has the amine in its tight little grasp and ate the better part of my yield from the Zyrtec tabs. Orange II had locked up much of the methamphetamine produced in the reaction of the pseudo I obtained from the zyrtec tabs and I cannot get the meth free of the orange stuff, no crystalization takes place, the shit just multiplies. 

This is the variety of Orange II I believe. The orange looking gakk in the reaction of the zyrtec tabs appears to be contaminated with the Orange II gakk. I think/ I will know next time to carefully a/b the pseudo from these tabs. Next time I extract from these pills I will sure as hell take the time to a/b the damn pseudo after extracting from the pills so I won't get that shit in my next batch.  will have another batch before long and will update the notes. If the a/b works, you will hear me brag about it.

See... that wasn't hard at all, was it?

(Note I made no mention of pints and drops were not employed in any explantion. )

The significance here is that it came through this process with the pseudo.

[wareami]

Geez: The OrangeII is a remarkable beast and a severe pain in the ass on the backside post-rxn a/b!
What's known so far is that:
1•It's solvent activated.
2•It multiply's and grows in basic solution
3•It's oily and hinders the formation of xtals.
4•It's a yield killer by UP to 50% of expected.

Just out of curiousity, What makes you think it isn't designed to rear it's ugly head in the frontside A/B?
It's obviously a Mo-Fo on the backside post-rxn A/B!
Ibee was able to recover 60% kick-ass meth from the rootbeer colored mess following a 30hr/100°C wet rxn but the dope was oily and wouldn't fully crystallize.
Although the crystal clarity of the final product indicated the absence of other impurities and a 4 day sleepless run  produced zero....zip....nada....black helicopters/shooting stars/other ill sides.

Peace of the _reaction

Have FUN-Bee SAFE

[mickyfinn]

The Orange II gakk only appeared in the third pull from the reaction fluid, which was done with xylene rather than hot naptha, and was allowed to sit in contact with reaction fluid overnight before being processed further.

Based on that being true if one were to optimize the first two pulls using VM&P or to pull all three with VM&P then, reasonbly, one should be able to elude the Orange II gakkattack. The third pull doesn't provide much anyway according to general concensus (at least, for bees who know the most effective drill and perform it correctly), right?

The significance here is that it came through this process with the pseudo.

SWIM would think that the significance would be that:

A)VM&P didn't activate it
  1.Xylene did...(what about hot Xylene?)
  2.Third pull did
  3.Third pull of room temp Xylene creates unique condition that precipitates O2gakkaTTack.

So "why" or "how" would be the next question for someone who understands chemistry.

[geezmeister]

The Orange II has to be avoided up front, pre reaction or you will lose yield, and lose heavily. I knew after the second natpha pull I had problems. The xylene did not pull the gakk, the pH of the solution going up pulled the gakk. On the third pull, after noting the low yield, I added additional NaOH solution as I knew I either had been gakked, or had a contaminant that interefered with the basic of the freebase meth. The higher pH brought the Orange.

That suggests it may be susceptible to an anhydrous A/B extraction of pfed at lower pH than 12.

The reason for posting this information in this thread is that the extraction technique this thread is about extracted this gakk with the pseudo. Xylene is not the problem.

[chronic_cook]

Would a steam distill pull the gak thru in the post rxn?

[mickyfinn]

The Orange II has to be avoided up front, pre
<snip nice simplification for SWIM, thank you very much>
extracted this gakk with the pseudo. Xylene is not the problem.

Okay, SWIM got his head wrapped around the issue now...gosh this forest is dense. SWIM was offline for awhile but will see if he can help Ware test the dot3 on his STE fred.

[chronic_cook]

Hmmm, well the og2 is defanitly oil-like. maybe that's why it likes fb ma so much? the RXN imho, makes the gakk one clever litter basterrd. It's rank shit that's for sure. the rxn has gotta change or activate the gak somehow, cause everyone started out with glass shards of pseudo, and rextl only AFTER the rxn really kicks it in the ass. swic noticed unusual rp tendancies in the og2 rxn. Like the rp was being eaten alive...pretty much making the reflux difficult but sustainable w/ some rp here & there..

[shaggy_day]

if you dry all your solvents it helps to stop the gakk also
when you are done with the whole prossess try to re crystalize with hot dry denatured this will couse a new thing to happen whin I did this it made a wax that was not found threw any of the previous steps to break off the psudo then strain crap off then let recrystalize once it is a crystal add more denatured to it .with a thin coat across the top scrape to make sure that it is all crystal becouse i found a second lair wax before i got a fine beautyfull crystal and i didnt loss much weight from 11.6 it went to 9.7 and it was clean and tasty once fired . also has anyone thought about methyl isobutyl ketone   and not mek that might be a better ketone to work with psudo

http://www.epa.gov/opptintr/chemfact/s_mibk.txt

Chicken head stricks again
thanks Kernal u helped us a lot

[chronic_cook]

swim did a STE extraction, dryed, rextlized w/ denatured for 5 hours,
boiled in natural solvent then crashed with dry acetone.

swim had good crystals. when he pulled the post rxn after settling the based aqua for several hours there was an inch of dark orange gak on the bottom.
No conventional STE methods well remove the gak if it is in there shaggy.

[halfkast]

Could one of the US bees do a small test to see if your VM&P Naphtha maintains its properties relating to its attraction to H2O molecules present in added IPA, when the aromatic hydrocarbon xylene is added to the naphtha before the IPA is added?
The best idea is to probably add hydrated IPA to a small amount of naptha/xylene.

It would bee really appreciated.

[spinhead69]

Pretty simple! I tried this and it works awesome. I showed my buddy a dish of it and he thought it was shit! Take a 20 oz. soda bottle and fill it with pills add water, shake it up and let the pills dissolve. filter the water. cook the water down until it gets thick. Let it cool. Add some lye until the pseudo water turns thick and almost solid like and filter the solid like shit out and keep it. Wash the yellowish crude with a litle water and throw it in very warm toluene and throw the solvent in the freezer over night.good morning you have pseudo crystals. rinse with clean solvent if you want. simple and works great. I hope I dont offend anyone, just thought I would give people an idea.