fearnoevil (Stranger)
05-21-04 23:33
No 508732
      Gooey blue pseudo - what's the cure?     

Hey Bees, Swif ended up with a gooey batch of pseudo that won'd dry after doing the alky pull on a batch of 60's he'd extracted with the TCE/JD method.  Now Wareami mentioned using Laquer Thinner (spec blend) to wash out the gakk that's causing this (over at WD) and now Swif can't find that info. 

Swif can't recall the details and hopes that Ware or any of the wonderfully knowledable Bees here can put Swif on track?
 
 
 
 
    ordinaryguy
(Stranger)
05-23-04 14:54
No 509103
      your gooey blue     

swim would need more info to guide you in the right direction such as a list of pill ingredients, swifs step by step extraction process that led to the goo to begin with. swim is aware of a cure all for these types of situations which is similar to pill chucking in a birch reduction called "goo be gone" but it involves NH3/Li reduction which is much more forgiving than a Rp/I or Hi reduction. If swif gives more info, swim may have a viable solution.

goo is only goo as long as you allow it to be
 
 
 
 
    fearnoevil
(Stranger)
05-23-04 16:01
No 509117
      Got Them Gooey Blue Pseudo Blues     

Hey Ordinary, well Swif did a TCE/JD extract (10:1 ratio of TCE and JD) on a mixed-brand batch of white 60's. Sorry don't have the inactives list. Basically just grind, wash with TCE/JD, then filter, dry and put the PM thru fine sieve. Then add denat alcohol and decant x3.  Now at this point you're supposed to be able to dry the pulls and then run xtals thru tone wash, but Swifs pseudo never dried, just formed a crust with oily stuff underneath.

Since then he found the info by Ware, which is to run the goo thru one tone wash then wash with lacquer thinner (brand containing: Petroleum Distillates•Methanol•Toluene
•Acetone•Methyl Ethyl Ketone•Propylene Glycol Monomethyl Ether Acetate•Ethyl Acetate•Xylene). This required a few steps and Swif wasn't sure he got all the gakk separated but the resulting PM dried nicely tho still slightly blue, so followed with 2 tone washes, then powdered for rxn.

However Swif may have screwed up cuz when he went ahead with the rp/I2 rxn it never acted quite right (well don't have any successful rxn's to draw on but other times initial rxn was always a bit violent at some point, but this time nothing really "happened", just bubbles and no cloud/smoke/genie.  Not sure if gakk can cause this or if Swif's rp was weak/bad. Swif'll post the whole debacle in a separate thread.

Swif would still love to hear your advice/info and thanks for any help for this newbie dreamer (still trying to get his wings, wink)!
 
 
 
 
    Scottydog
(Hive Addict)
05-23-04 16:42
No 509123
      Recrystallization helps to rid blue oil     

Blue 60's with clorpheniramine maleate...right?

Recrystalization alternating between ISO IPA and dry acetone will do what the LT does. Ditch the crust that forms on the sides; it is gakk. Deal with what forms at the very bottom, isolating IT from the oily gakk that forms the crust.

Might take 4 reX's to get the crude pseudo to the point where it no longer releases any blue but somehow Swim has a feeling that Fester's cure (with 91% IPA and KOH) could bee employed immediately after a majority of the oil is gone.

*Enough oil is gone to where the pseudo will half-ass dry/ No more of it can freely bee decanted*

Swim kind of has an idea of where you are at. Pseudo that you feel may not have released all of the blue oil may bee residually gakked. Knowing this, Swim has also found that by using more I2 and RP then one normally would really helps because this gakk will stall a rxn.

Swim uses hypo and has found that sometimes not all of the I2 gets converted to HI so he will reflux until no more activity, add more hypo and reflux a few more hrs until it does. (Enough until the solution goes from red to yellow) Don't know why but it seems to work for Swim. wink

Swim does not mean that by rushing the extraction and avoiding the recrystallization steps and substituting the extra precursors is the answer either. This gakk encapsulates the pseudo and the reX steps will result in a loss of yield. 

Have yet to try Fester's cure but has a hunch that it could bee used as a finishing touch just prior to rxn.

Or maybee Fester's cure could bee used much sooner in the extraction, before decanting a majority of the oil because this blue oil is most likely the shit that forms the bottom layer (that Fester refers to) after refluxing with KOH and 91% IPA?

Anyone?

Edit: Another bit of crucial info. It is best to reX to get as much of the blue oil out prior to rxn because not only will it stall the rxn but if combined with excessively high rxn temps will also fry the pseudo before it gets a chance to convert to meth. Alot of you bees putting in 30+ gs of pseudo and getting back 5 to zilch gs of iodo/aziradine know what Swim is talking about. frown

Refuse/Resist
 
 
 
 
    weaz1dls
(Hive Bee)
05-23-04 17:08
No 509126
      Here ya go     

Post 486908 (weaz1dls: "Oops grabed the wrong solvent, think again!", Stimulants)

Be aware that laquer thinner will disolve your pseudo.  Wareami used it to rinse and save wash.  It is kinda like rinsing your final diamonds with a mix of acetone and alcohal 80/20.  The low presence of alcohal will wash the surface clean.   Plug in Wareami and blue or wareami and jap in the search engine.
 
 
 
 
    fearnoevil
(Stranger)
05-23-04 17:10
No 509128
      UH-OH.....     

Hey Scotty, thanks loads for that - Swif expected some of this and wondered if a gakk could actually stall the rxn mad.  The uh-oh comes in cuz Swif has already run his rxn last nite (see "No reaction in my rxn" post) and there were some high temp moments so yields might be low if at all, not sure what limits we're talking about tho. When the cook was done had two bad/strange signs - chili smelled more like chemical/petro/oil, not fishy and there were what looked like PLASTIC beads mixed in with the rinsed RP!!! Rxn fluid, after filtering looks liked water, maybe very faint color, but Swif thinks he's screwed, grrrr.  Thanks again, always look forward to your input smile!

Oh yeah about 1/3 of the pills contained the clorpheniramine maleate - those are the culprits???  Are there ANY pills still safe from these grim reapers, lol?
 
 
 
 
    Scottydog
(Hive Addict)
05-23-04 17:35
No 509134
      Excessive NaOH Necessary     

there were what looked like PLASTIC beads mixed in with the rinsed RP!!!

Actually it may form a clear to rootbeer colored layer that falls to the bottom of whatever glass container you will use to do the basing. Excessive NaOH will bee required to get the freebase to migrate into the NP. Most likely to the point of lye-lock. tongue

Also you WILL KNOW by the multi off-colored NP one gets after basing with NaOH. These colors will not transfer to the polar upon titration. But you will know youve been gakked by the blues and greens. When you get this high sign, bee prepared to literally dump in the NaOH.

The gift that keeps on giving...Eudragit TM! crazy
 
 
 
 
    fearnoevil
(Stranger)
05-23-04 17:48
No 509139
      Thanks for that link weaz1dls - excellent info     

Thanks for that link weaz1dls - excellent info for future ref!

Scotty,
So are these plastic beads (they really do feel like rubber/plastic) actually contain product or gakk or both? And sorry for Swif's density but what will "form a clear to rootbeer colored layer"?  Yeah Swif's still a little rummy from the late nite ordeal and then working on 4 hrs sleep without the aid of better chemistry, lol.
 
 
 
 
    Scottydog
(Hive Addict)
05-23-04 17:56
No 509141
      The Rootbeer Layer     

Swim has yet to see these plastic beads in the rxn that you speak of. The gakks that transfer from the residual blue oil to the post rxn workup are usually invisible and not detectable by sight in the actual rxn itself.

It is upon basing that he realizes he has received a gift. crazy

Refuse/Resist
 
 
 
 
    wareami
(Hive Addict)
05-23-04 19:32
No 509149
      Eudragit Oil Fields....     

SWIF must not have been SWIFt enough to catch the reply at Wetdreams this morn before the work-up.
A shift in cook times toward the 48hr mark would have helped immensely.
But that didn't happen.
Let's back up to the point of extraction.
There are three key solubility issues that are addressed in the Eudragit Documents.
In order to effectively employ any workarounds toward ridding the oily substance that hinders drying in the extraction stages, it's important to review those pdf docs that were posted here in the thread Post 494861 (wareami: "Eudragit", Stimulants)
Pay close attention to the solubility data.
Eudragit and Eupergit can be defeated.

Now...SDawg brings up a scenario that details rootbeer colored basified solution. This strongly hints at the effects produced by orangeII gaak.
OrangeII gaak is still alive and well in some brands.
OrangeII will fall by the wayside if a properly ratio'd JD/TCE wash is employed. Emphasis on the ratio...
10:1 TCE/JD
Many make the mistake of thinking the anti-histamines are causing the problems with the blue that won't go away.
Make no mistake here....this blue is the heavymetal imparted to the pfed xtal by the JD.
This blue needs to be removed or the gaaks will still be present.
If eudragit is employed, it hinders the removal of the blueness(heavymetals).
Two known workarounds here when this happens.

•Add 5-6 drops HCL to the tone while rinsing the xtals after they are evapped and scraped up.
•Charge the alcohol with HCL prior to the alky extract/filtration/evap.

These 2 workarounds only address the removal of the blueness.
They don't remove the oilyness or the gaak causing it.

Resourcefulness is required when aquiring the lacquer thinner as they have changed the formulation and only the old formulation will work as prescribed because it contains the only ingredient they excluded in the new formulation.

With these gaaks present today, if doing an HI/RP and these gaaks cannot be removed completely, the best chance at success will rely on the patience of employing a LWR.
Too many bees are getting screwed by these gaaks when they attempt fast/hot rxns.

a little less conversation, a little more reaction
 
 
 
 
    weaz1dls
(Hive Bee)
05-23-04 22:11
No 509174
      Petro smell     

SWIW has noted this smell also on rxns run after JAP-TETRa cleaning.  The pills you speak of will fool the eye my freind.  Pseudo  in it's pure form will not form such beautiful geometric shapes without a builing partner. There is the natural formation of paterns and there is the jaged formation from the modern museum of gack.  Which did you have.  These pills have been run with sucess using the same technique for the 120's SWIW posted, both alone or mixed together.  SWIW opts for the 120's.  Less trips down that isle.wink
 
 
 
 
    weaz1dls
(Hive Bee)
05-23-04 22:24
No 509175
      Down to the last drop..     

Scotty following Scotty's sugestion SWIW would like to steer you to the search engine to plug in "Kerplunk".  Also if heating th mix in the microwave be careful for it is the np that wil get hot real fast here.  Heat and mix heat and mix, use this to you advantage with naphtha. Do 6 pulls with small portions each time adding more Naoh.  Combine the pulls. Rinse once with a small bit of Dh20. Do not vigorously wash.  Naphtha is picky and needn't be washed like a rakoon meal. good luck!....oh one last thing, when ya dry out the titration add acetone at 3 times the volume when it reaches the syrup stage.  Boil in the micro and continue the acetone addition till the stuff becomes anhydrous and comes out in the boiling tone.



Edit... Sorry Ware did not see your ref to kerplunk... Never a suprise that we think alike here as we obviously share similar experiences!laugh
 
 
 
 
    wareami
(Hive Addict)
05-24-04 05:29
No 509228
      Steam distill...     

Weaziese Master:laugh
With eudragit, while it tends to lock up the amine when doing an acid/base extraction, trying to force the amine over via kerplunking seems to force the oily gaak over as well. Not saying a kerplunk won't work. Just saying the end result will still be tainted. Granted....a few re-xtallings or a few tone washes will clean the end-result up some, but the properties and behavior of this new gaak seem to make both pfed and the meth amine more soluble in acetone for some strange reason. Don't know if other bees have noticed this but Ibee's experienced it.
Since this eudracrap hit the market, when it's found to exist post-rxn, Ibee has been extremely successful with opting to steam distill instead of a/b.
He'll do an initial a/b to determine if eudrigit made it through rxn and if it has, he'll steam distill the rest.
Less muss....less fuss....cleaner end result...less chems needed and faster than kerplunking as well.
So steam distilling wins hands down when faced with gaaks post-rxn.
IMHO
More testing is needed on identifying this seemingly invisible gaak.
It sure is a bitch when you think you've removed it pre-rxn and it rears it's ugly head post-rxn!
Waiting it out works some with a/b but just as the case with kerplunking, the gaak comes with the amine.
Also some tests are underway to tame or capture the gaak with polar solvents during the basing stage.
Nothing solid yet.

a little less conversation, a little more reaction
 
 
 
 
    ordinaryguy
(Stranger)
05-24-04 08:43
No 509264
      gooey blue blues     

From reading the additional posts you have recieved on the subject I would say that they've narrowed it down. The one and only thing I could add, which may have been stated already, is that it most likely is from a metal contaminant and as with any contaminant should be cleaned out prior to using the E in a rxn. If not, it most assuredly would follow to the final product and may have adverse affects on the rxn itself.

The only blue I like to see is the True Blue in a NH3/Li rxn