Author Topic: Blue to Green to Brown RXn Fluid  (Read 4887 times)

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tina_craig

  • Guest
Blue to Green to Brown RXn Fluid
« on: September 29, 2004, 06:24:00 PM »
With each addition of 20% lye mix to post rxn fluid the color went from blue to green to brown.  Is this normal or what the hell?


geezmeister

  • Guest
it could be:
« Reply #1 on: September 29, 2004, 06:50:00 PM »
1) lye, rather than NaOH
2) polymers still in the pseudo that are in the reaction fluid.

Both can cause the effects you mentioned.


wareami

  • Guest
Layered gaak!
« Reply #2 on: September 30, 2004, 12:42:00 AM »
Don't expect crystals from the evapped goodz...what little you're able to pull.
After letting the basified solution(BS) set 24hr+...the encapsulators should settle out.
The quick work-around that seems to work best in cases like this is a steam distillation.
If NP was added to the BS...pull the NP and titrate or gas.
Then steam distill BS.
Chances are...if the BS is brown(rootbeer color), the pH was overshot which activated the OII gaak.
The blue then purple was OI gaak.
The oil in this case is either a combination of eudragit and polysorbate60/80...or just polysorbate if the pills predate the inclusion of eudragit.

The experience is the result of gaak layering with multi polymer/co-polymers trained specifically to interfere with the precursors, effect pH before/during/after rxn, effects dissolution, and inhibits crytallization.
This gaak layering, it seems, was introduced in response to the previous failed attempts at preventing extraction of the main excipient.
Their take is this:(my opinion)
"We can't prevent extraction effectively! (Do we even want to? It would crush pfed sales!)"...
"We can't stop the bees from getting to the goodz...
At best, we can make the end product unappealling and unsellable for all at the street level, but the most skilled!
At worst...we'll make a bitch and half"

Not long ago it was possible to eyeball solvents and extractant aids.
This is no longer the case. If one solvent is skimped on that is aimed at solvating or disabling/deactivating a particular gaak, you've stopped short of a successful extraction and will run into problems.
Precision Gaak requires precision technique.
In his Deconstructionist Thread, Uncle Fester recently touched on a subject Ibee has been hounding about for years.
Most will take the quick/logical approach of attempting to get the pfed out of the pills. Most all of Ibee's extraction methods, that proved the most successful, centered around getting the crap out of the way and then you're left with the goodz and some easily removed binders that a simple solvent wash deals with!
It's a simple mindset switch...but makes all the difference when approached from that angle.

Since precision is required, it's necessary to develope trial and error test batches...depending on the extraction method and suggested ratios.
Something as simple as saying 7-10 parts ethanol to pillmass volume is enough to screw ya...
Too much, pulls gaak...too little requires extra pulls that pulls gaak.
It's the Old QuarterTurn NutCase syndrome Geez used to describe plumbing leaks or was it gasket-cases? :)
Either way....Ibee's take on the described scenario:
SWIT_C got triple gaaked...something bees will see with more frequency if they don't focus their energy and time on the pre-rxn cleaning.
Also not too long ago Ibee could have said(and did say) that it was more time efficient and easier to deal with the gaak first before the rxn than it was to deal with the gaak in the difficult work-up post-rxn.
That statement would be false today because both are equally a bitch and both require many steps to get to the goodz in an eye appealing, consumable end result.


tina_craig

  • Guest
Pill xtract
« Reply #3 on: September 30, 2004, 04:58:00 AM »
swim used festers KOH boil extraction technique.  swim evapped my water pull from toluene extract and pulled acidy salty meth which swim washed with tone to reveal sparkly white gogo.


wareami

  • Guest
Yield???
« Reply #4 on: September 30, 2004, 05:10:00 AM »
Being the E-tern-AWE optimist...
How bad did the yield suffer? ;D

Luckily Polysorbate was not one of the layers since SWIM didn't have xtalling problems, but Ibee ran into recently in the newest formulation, leaving him scratching his head!


tina_craig

  • Guest
The Battle of Mt. Gaak (Attack of the polymers)
« Reply #5 on: September 30, 2004, 06:07:00 AM »
Yield loss may have been swims own fault, the general sent in 9.45 soldiers and only 3 returned.  They were attacked by the KOH battalian led by the 450ml 91% ISO IPA calvary.  Attacks were made by the KOH infantry right at the calvary's boiling point.  After attacking for 30 minutes the soldiers were cooled and the living were decanted off of the dead and and their bodies were drained of all fluid through evaporational means.  Then they were covered in tolly fluid and impatience became a nuisance so gas was introduced early and probably suffocated some of the living.  So, the commander in chief ordered a evap of all fluids and a combination of forces from water and tolly were combined.  Produced some soft fluffy soldiers with a slight tan.  This was used to plan the final war tactics.


geezmeister

  • Guest
please consider...
« Reply #6 on: September 30, 2004, 04:34:00 PM »
Ware...please consider, as I have, that any particular product could have multiple approved formulations which are rotated by lot number, each formulation having a slightly different blend of polymers from the other lots, each lot with slightly different solubilities, enough that an extraction method that works with one formulation does not work with another.

This explains what I have seen several times over the last few months. Granted, there may be other explanations, but when a method works with one lot and not the next, then works again with a later lot, the successes and failures suggest that the foilants in the pills may be different from lot to lot... at least on the pills I've worked with.


wareami

  • Guest
How Right You Are!
« Reply #7 on: September 30, 2004, 07:35:00 PM »
Geez, the facts you state for consideration have been my experience as well! Perhaps I did jump the gun with an all inclusive assessment of what bees are faced with. I see this now in retrospect.
In the midst of my own frustration, I find it hard to ignore this gaak progression based on the writing on the wall.
Not all bees will encounter the exact same formulation at the same time, which throws any individual assessment off kilter slightly.
So for me to have drawn definitives from the described observed visuals was wrong. :o
Yep...That's right folks....you read it here first! :P  
I said it! ;D
When all this comes full circle and all the gaak testing and inclusions are given the green light, I've presented a likely scenario to be the root cause.
These individual gaaks are being layered in combination, as witnessed by Ibee, and I'm sure SWIG as well.
This is the steady progression that has been in effect for two years making the next box/lot# harder than the last.
Then up pops a box that comes through with flying colors...almost water extractable in some cases.
Now that may be the edge they're employing as the means to make a bee let down his guard long enough/often enough to wipe out of larger percent of their successes. Thereby boosting OTC sales while reducing the amount of finished product.
All in All, during testing and devilopement, Ibee's trashed more pfed than he's reacted. That's to bee expected by any pioneering Do-Bee!
But the sacrifices have provided relief for a time to many bees so it was well worth it!
The predictable tactics are infinite, but the logical progression and patterns are the ones Ibee tries to predict as the area to look for next, soas bees aren't caught completely off guard.
I also wanted to express above that there are best case scenario's that should be employed regardless of the pills/gaaks being encountered.
Uncle Festers KOH method is working wonders for many that go that route.
Prepuce and evilscripter's routes of extraction are also very promising across the board on all strengths.
Some still use algreich's TetraTrap Method and variations thereof on the 120/240's.
Those that have mastered the elimination of the Heavy Metal residue when using the Slanted Egull Method are still reporting successful extractions on White 60's in high yields.
Even The Geez Waterless a/b and placebo's Turps Cure is reportedly successful by themselves in some parts of the worldbee colony.
And when all else fails and something slips through rxn, we have an abundance of baseline practices in TFSE® to skirt around the hedious gaaks to get at the amine post-rxn.
However, the latter practice is becoming a threat based on the toxic characteristics of some classified inactive components that may or may not bee health hazards if they skirt around your attempts and pull UP your skirt instead winding up in the finished gear. :-[
The jury is still in deliberation on that one, but it's something serious that shouldn't be overlooked as a possible suspect in the LINE-UP!

So instead of looking at my above post as the definitive cause of individual adverse encounters, I'd prefer bees use that info as a base troubleshooting guide to refer to as these cases start becoming more frequent.
And to see this post as the signpost that is predicting the wave of things to come when these international pharmceutical community establish the all inclusive "Wham Bam Thank UncleSam"!
It will come once they get their ducks in a row.
The way I see it is, when they feel that 50% of the OTC remain extractable, they have more work to do and won't accomplish their main goal until all makers are brought to the same standard that is most effective.
That layering gaak encountered, as described in the above post is just that beast!
The patents that aren't redacted by TradeSecret disclosure are out there and they are all we have to draw reasonable conclusion from.
There is a hiccup effect going on, and rightfully so.
They need to deliver the final blow when the dissenting votes are outnumbered by the consenting.
In the meanwhile...I believe what bees are seeing, is there is a trickledown testing approach that must be deployed to gather the effectiveness statistics data at stopping what they deem to be a major problem.
In the undersirables eyes, Pfed is not the only threat! Many other extractable main excipients in pill form,(OTC and Prescription)are far more harmful to health and life in stronger concentrations.
So We should reasonably expect things to get worse before we ever see them get better.
I'd prefer to be seen as a paul revere type than a boy who cried wolf type. Either way, I live out on a limb, so it's unlikely I'll ever get the chance to bury my head in the sand on this subject.
"Inactive" has left the building!
"ENTER THE MATRIX"
That occured with the advent of the DryMatrixFormulation and it's been an UP hill battle ever since!
So exacting that a bee could set his clock by it!
So as Geez says...approach each extraction with caution and like a box of assorted chocolates...and never ever put all your eggs in basket! :P
Thanx for smacking me around some Geez! ;)  It keeps me on my toes! ;D


tina_craig

  • Guest
So what does all this mean?
« Reply #8 on: September 30, 2004, 08:32:00 PM »
I was still able to pull some final product from the final mix.  Are these here just to make the final rx pretty?  These pfeds were as generic as you could get, 13 boxes of 2 different brands and they were pretty loaded with inactives.


wareami

  • Guest
Nope...
« Reply #9 on: September 30, 2004, 09:16:00 PM »
The final product recovered indicates that reduction took place...This doesn't necessarily mean that the reaction was 100% gaakfree or 100% successful.
The simple facts that lead to the posting of this thread were always signs that Gaak made it through the pre-rxn, survived the rxn, and could possible have become part of that final product.
This is the "walking on eggshells" part of not analytically determining the meth's purity/impurity.
The classification of two of three main components that eudragit are comprised of being "MUTAGEN" raises a large degree of concern in my eyes when I see posts where others may not have rid those specialty co-polymers in the frontside cleaning.
The yellow oil is the surest sign they are present!
The OI and OII gaaks being layered in, presents what may be a masking of the eudragit as these are encapsulating gaak.
Again...with no definitive experience in analytical chemistry, bees are at the mercy of guesswork when anything but normally observed work-ups are encountered.
Until the facts come in that determine eudragit infested final product is not a health hazard...you'll see Ibee chiming in with ways to skirt around it and links back to these warnings for bees to draw their own conclusions as it's their health...therefore....their call!
If you're not sure what exactly you have got in the end....you are not sure that it won't harm your health or others!
The only way to know aside from professional purity testing, is by making sure that first:
•The starting feed extracted from the pills is on par visually and yieldwise and relatively free of the known gaaks...and secondly:
•the work-up goes exactly by the book with no sign whatsoever of gaak!

The colors encountered during work-up in this case suggest that gaak made it through the rxn.
At worst...the endproduct is tainted with gaak
At best...the work-up is just a bitch and the encapsulating gaak settles out in the BS and doesn't steal too much yield in the process.


tina_craig

  • Guest
So is color a good indicator?
« Reply #10 on: September 30, 2004, 10:15:00 PM »
So since the nasty colors remained in the BS and the gogo did come out crystalline and white does that mean the final clean was successful?  Nice how they think they are improving society by selling poison laden shit!!


tina_craig

  • Guest
24 hours later.....
« Reply #11 on: October 01, 2004, 01:33:00 AM »
swim returned home from work today to find his reaction fluid had cleared considerably. swim left a layer of xylene sitting atop the fluid all day and now there is a slightly murky rxn layer a thin layer of brown gump on bottom.  swims ? is, will this xylene layer contain any product?  swim pulled until there was nothing left with naptha but since the crap has settled has it released anything?  Here is a pic of what swim is talking about:



geezmeister

  • Guest
try it...
« Reply #12 on: October 01, 2004, 04:11:00 PM »
Try it. I always leave my reaction fluid sitting for at least a day with xylene over it. You'd be surprised how many times you get a little more meth.

This doesn't hold true if you steam distill, by the way...


wareami

  • Guest
Rootbeer Float!
« Reply #13 on: October 01, 2004, 05:14:00 PM »
Well...now the newbees have a clearer picture of the rootbeer float syndrome caused by the notorious OrangeII gaak in most cases!
If left to sit 1 or 2 more days that brown will settle completely out. Ususally it falls to the bottom.
If there was a large emulsion it will sometimes attach to that and be floating on top.
This is why the initial recovery suggestion was to steam distill. The orange II gaak is not volitile and the rolling boil will loosen it's grip on the goods.
SWIT_C could have had all the goodz in under an hour.
The second optimal scenario is waiting for it to settle out.
But since that can take daze...
C`mon now?.....we're dealing with bees! ;D
But SWIT_C must have the patients of saints! 8)
Good Luck


geezmeister

  • Guest
it also helps...
« Reply #14 on: October 01, 2004, 05:56:00 PM »
to heat the reaction fluid with the xylene on top, creating convection currents in the fluid, so that it all contacts the xylene as it moves. When the xylene is hot, let the mix cool, decant or separate off the xylene, wash, then gas or titrate.


tina_craig

  • Guest
48 hours coming soon......
« Reply #15 on: October 01, 2004, 06:56:00 PM »
swit_c will see if anything can be recovered tonite.  swit_c will post a new pic if fluid appearance has changed dramatically so there is a 24 hour and 48 hour reference.  Back later with results!