Author Topic: Problem gassing generic 120's  (Read 13760 times)

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lugh

  • Guest
Column Chromatography
« Reply #20 on: March 04, 2004, 08:07:00 PM »
Here's some more basic information on oolumn chromatography, as usual lab equipment is best, but the imaginative bee will realize that such a column could be improvised from materials they can scrounge up  ;)



8)


geezmeister

  • Guest
I see the future
« Reply #21 on: March 05, 2004, 12:18:00 AM »
I get the hint. I think I see the future. At least mine. I believe its time for this old dog to learn some new tricks.
I'm still willing to learn.


CharlieBigpotato

  • Guest
jumping up 2 steps
« Reply #22 on: March 05, 2004, 03:56:00 PM »
gotta admire the old dog spirit, but, by the time sophisticated analysis and seperation techniques are learned for shitty pills, they won't bee available at all.

may as well jump ahead to what lies beeyond the pills.

8ball

  • Guest
Tryed again....
« Reply #23 on: March 06, 2004, 01:46:00 PM »
After trying again with 5 boxes of 30x60mg name brand whities my results were even worse, but i take the blame for that because instead of soaking in np for 12 hrs i went for 6 hrs(waterless a/b). At least this time it gassed but still took 1 1/2hrs to get everything i could and what i got was a pile of sticky goomp. After pouring about a litre of acetone from the freezer through it, it was a little better but not much, so i put the sticky goomp into a 1000ml pyrex chem bottle with approx 400ml dry 99% isopropyl brought to the boil and then added 400ml dry acetone and brought back to the boil, then capped and left to cool to room temp then fridge then freezer. Me being a nosy fucker i didnt leave alone, i shook it and whatever before filtering and ended up with a dirty sticky ball of goomp for pseudo so i rinsed with fresh cold ace(all my solvents are pre dryed) and set aside. The ace and iso i used to rextalise was returned to freezer to see what else would evolve this was 2 days ago. today i checked and to my surprise the chem bottle had pseudo crystals stuck all up the sides of bottle, mine normally settles as a soft blanket in the bottom. After some serious shking of bottle i managed to dislodge the xtals.  These crystals were like little 3 and 4 prong prickles. All up i recovered 3.3gms of pseudo out of possible 9.
i think with full 12 hr soak and more gassing or should i say use a lot more np in the a/b to gas the pseudo in. My feeling is maybe this sticky goomp gak saturates the np making it more difficult for the pseudo to be gassed giving it nowhere to go making it bond back onto the pseudo following it all the way through. IMHO i feel the amount of np used in a/b needs to be doubled if not tripled the amount supposed to be used already and likewise with rextalising. I only rextalised the once then returned iso/ace back to freezer to sit for a couple of days and was stoked to see what happened in my absence.
I have kept some of these aside(xtals) the rest is bubbling away at the present, so if anyone is interested in telling me how to upload picture step by step i will post one. I had a look at the upload page and sorry i'm not really computer  literate enough to understand properly what i have to do. Xtals are small even minute but they are xtal clear and do not cling together.


gluecifer69

  • Guest
seems you got clean product there eight ball.
« Reply #24 on: March 06, 2004, 07:08:00 PM »
seems you got clean product there eight ball. :)   Swim doesn't know why more bees are using ScottyDog's method.  Gluecifer knows that it works on the 24 hr pillz because swim smoked the meth from them and found it to be up to par!  :o

Gluce hasn't even fucked w/ the 120s this week. :(


8ball

  • Guest
Tried again.........
« Reply #25 on: March 09, 2004, 10:04:00 AM »
Heres that picture of clean pseudo. Recrystallized once.



Rhodium

  • Guest
Online Publishing 101
« Reply #26 on: March 09, 2004, 10:13:00 AM »
Could you please crop out the interesting parts of the picture? I don't think anyone here wants to download a detailed picture of your kitchen bench.


ClutchCargo

  • Guest
Another excellent chromatography reference
« Reply #27 on: March 20, 2004, 08:58:00 AM »
Have a look at

http://www.chem.cuhk.edu.hk/labtech/index.asp

. Among other topics, there are videos on column chromatography. They are dubbed in English, but those who speak Mandarin may get even more from the experience.

Clutch

ClutchCargo

  • Guest
You gassed and got freebase???
« Reply #28 on: March 20, 2004, 09:11:00 AM »
Scotty,

You write
> C) Gass out the freebase (Which should really bee pseudo HCL > but isn't)

Is this what you meant to say? I think I know the answer, but how can it be? How can it be that you gasased with HCl, I assume, and ended up with freebase?

Clutch

Scottydog

  • Guest
Takes on FB-like properties after gassing
« Reply #29 on: March 20, 2004, 11:27:00 AM »
CLUTCH  Yes, exactly what I said. Swim gassed and got freebase! With the generic 120's, after gassing to the point where nothing more will precipitate, upon adding this crude pseudo "substance" to water and xylene and shaking it up, most of it will float on top of the water.

After then doing a ph test of the water, he got a reading of 10. He believes that it falls out of the solvent at a ph of 9-10. Why it is suddenly doing this, he has no idea but whatever it is, he believes may have something to do with this new gakk.

After all, if it was pseudo HCL, with the amount of water added, it should have completely dissolved in solution.

It requires an additional titration step with HCL acid to get the pseudo salt.

If you don't, well then you are stuck with yellowish paste.  :P

Edit: Swim has narrowed it down to 120 pills with a 07/06 expiration date. These have a new font on a more difficult to open blister pack (thicker foil/plastic)

Swim also noticed on the perrigogo 60mg pills they also have this NEW font, could it bee that these possess the demon as well?  ::)


ChemoSabe

  • Guest
Chemical identity Crisis
« Reply #30 on: March 20, 2004, 02:01:00 PM »
Swim's buddy who can somehow legally mess around with such things passed me this note.

I've noted this same type of behavior in both extracions of psuedoephedrine and in the final reduced product and for lack of any better terminology have been signifying it with the term "chemical identity crisis". Which seems to have the substance in question not being certain if it's a freebase or a HCl salt and under differing environments displayig varying characteristics of both. This, among other things, makes final cleanup and purification by usual means a challenging and as-yet-unresolved process.


UncleFester

  • Guest
complex formation
« Reply #31 on: March 22, 2004, 03:15:00 AM »
This sounds a lot like something that complexes with and ties up the free base. If that's the case, then on a chromatography column, the product would be stuck to and ride down the column with the gak. Just speculation on my part, but it makes sense.

wareami

  • Guest
Noticible differences...
« Reply #32 on: March 22, 2004, 05:35:00 AM »
There will be many noticible differences to come.
The products they are incorporating as inactives, which coincidently are not going to be considered inert or inactive ingredients because they are part of the delivery system, have a shorter shelf life than all the previous inactives!
A few months ago it was relatively common to find 08 exp dates. Then all of the sudden this new gaak hit and now the dates are back down to 05 and 06.
Now we all know that they will pull stock on a secret recall basis everytime they unleash a new foilant.
Worlock was the first to advise keeping a close check on those dates and lot #'s.
When shifts are noted, then it meant trouble on the extraction front.

This delivery system thang kinda sux because it opens the loophole in their favor in regards to "Consumer Right To Know" labeling and non-disclosure if separate permissions are applied for and granted throug the FDA.

Almost two years ago Ibee started a Pill ID/Lot# chart at Chemhead in an effort to develope a system to combat certain gaaks.
It became a monster to keep UP with but alot of the complexities that surfaced taught us much.
We are at a stage now where the lot#'s and expiration dates are crucial to identifying what is included.
After much thought however, Ibee wondered if revealing this crucial data might somehow be reflected back on an individual poster by zeroing in on region or locale.
It's still not known and hence may not be the wisest move.
At present we've gone solely on characteristic behaviors of these gaaks as identifiers and until something consistant and more concrete is known, we'll have to rely on small batch testing to reveal what works on which pills.
Now in regards to lot#'s and batch composition, there may be a further hinderance in identification which may include multiple formulation spanned over whole lots which may taint large batch extraction.
Remember, a little of that shit can go a long way at tearing down the sought after if allowed to travel through extraction and make it's way to the end.
It's those resilent gaaks that they mark and target to avoid detection so they can sidestep even the most thorough extraction methods. Be it through encapsulation or coating, it's very nature and design is to remain one with the main excipient.
This reminder is only to drive home the importance of "Separation and Removal"
That separation process now involves a deactivation step that wasn't necessary until orangeII gaak hit.
Ibee thinks they flipped the switch on this new gaak that now gets activated instead of deactivated when exposed to the same solvents that commonly deactivated it before.

It's relatively safe to bet that there is no such thing as a Universal Cure anymore nor can one bee expected.

But...if it takes five lesser cures to effectively deal with the multitude of denaturants and adulterants until the pills are no more...then by god, the bees will deliver the necessary blows!

"Every mistake We must still be learning....
While My Guitar Gently Weeps"


CharlieBigpotato

  • Guest
detergents might bee fun
« Reply #33 on: March 22, 2004, 07:32:00 AM »
wareami,

my friend, i was wondering if your efforts toward cleanliness had ever brought you to detergents?

i feel a wash-day miracle.


Rhodium

  • Guest
Amphoteric polymers
« Reply #34 on: March 22, 2004, 04:41:00 PM »
[I've] been signifying it with the term "chemical identity crisis". Which seems to have the substance in question not being certain if it's a freebase or a HCl salt and under differing environments displayig varying characteristics of both.

The proper term is "amphoteric" and is applied to compounds having both acid and basic groups. Take the amino acid glycine for example:

NH2-CH2-COOH

It has both a basic amine group and a carboxylic acid group. At very basic pH the acid group will become a carboxylic acid salt, making the compound soluble in polar solvents (water, and to some extent alcohols), and if the pH is adjusted to acidic the amino group will instead become protonated (= becoming an amine salt), also making the compound soluble in polar solvents.

It is just at a narrow pH range (usually close to neutral) this compound will be a freebase in the amino end at the same time as the carboxylic acid end is in it's free acid form. This is called the isoelectric point, and for glycine it is at pH 5.97. Depending on the molecule, this isoelectric point will be at different pH's, so imagine what would happen if they made a polymer with various different acid and basic groups on it, so that at any pH some of them will form a salt - there you have your polymeric gakk behemoth molecule slimying around your pseudoephedrine molecules, impossible to wash away.


geezmeister

  • Guest
dreaming about lot numbers
« Reply #35 on: March 22, 2004, 05:16:00 PM »
A couple of us detected Orange I gakk recently in pills that had not had Orange I. These had previously had OII.
It occurred to us that as the extract approach differed from OI to OII to Eudashit, the companies may be compounding extraction by rotating batches with OI,OII and Eudashit in lots, so you never know what you have until you extract it.

Which means you do a test on each lot number, or you extract with the assumption that all three gakks are present.

I actually dreamed about recording lot numbers and listing which gakk was in which the other night. I woke up moaning about the the added steps that a cover-all-the-bases cure  took. I can't say there is any real information to support this concept, or enough to even warn about it. It might be wise for each of us to look for the emergence of one of these three gakks when least expected-- for that could indicate if the gakk swapping by lot number is also something else going on that gives rise to more frequent lot numbers.


Osmium

  • Guest
> the companies may be compounding ...
« Reply #36 on: March 22, 2004, 05:38:00 PM »
> the companies may be compounding extraction by rotating batches
> with OI,OII and Eudashit in lots, so you never know what you have
> until you extract it.

If that is true then a little THIN LAYER CHROMATOGRAPHY (there is that evil c word again!) might help you in deciding which one is present.


UncleFester

  • Guest
amphoteric polymers
« Reply #37 on: March 23, 2004, 12:43:00 AM »
If this was all there was to it, they would act as buffers, and when hit with a gassing they would all be in their acid state, or with xs base, they would all be in their base state...and the weaker base sudo or ephedrine couldn't compete with the strong base NaOH for spots on the polymer, or when gassed, the HCl should preferentially be absorbed over weak acid sudo HCl. In any case, an excess should overwhelm its buffer unless there is something more sinister involved...
I would like to add a further observation to the already excellent physical properties listed on this thread...
When the new pills are extracted after clean up and then gassed, the precipitate and left over solvent(toluene) are more unmanageable than I have ever seen. Rather than filter,
if the gassed toluene is then extracted into water, and after separating the toluene the water is based, crystals of sudo don't appear with Na2CO3 as basifier.
The best methods are always the simple ones. Chromatography will never be teachable to the masses. For this to remain a people's art, a simple and effective method of knocking out all the new adds must be pursued. I'm putting my bets on superheated steam. Regular steam distillation of ephedrine is borderline workable, and with sudo it just sucks. I'll bet steam hotter than it wants to be will carry the product out without wondering if the product in the pills is Orange Gak 1,2 or 3 or Eudrashit...and I'll bet it can be done on a stove top.

UncleFester

  • Guest
this new shit continued
« Reply #38 on: March 23, 2004, 01:52:00 AM »
Just thought I should add...when the Na2CO3 sat water was hit with NaOH, the most wonderful looking(I emphasize looking) flakes of pseudo free base fell out. This was with an orange looking original gassing. If this was all there was too it, it would just be another day. The orange shit stayed in the water. Has somebody discovered this already??
I should read more, but the kids want me to play so my screen time is limited...

CharlieBigpotato

  • Guest
bizarre find
« Reply #39 on: March 23, 2004, 03:09:00 AM »
swim hasn't dreamt a little dream since the one that was over-the-top agrravating and bad yielding; the same one that never did allow a pristine end crystal.

it had been months. swim is seeking a stim; decides, in the spirit of futility and shameless addiction, to mine the mbrp left-overs for a possible line .

this was a 3gm rxn, and swim had already rinsed the rp with boiling water post rxn.
this was a desperate act, like going thru a trash can for an old ciggarrete butt.

anyway, with the crassest chemistry known to man, and no washes, swim evaps down the water to find some gear that was far cleaner than its mother rxn's end product, with 6 washes; acetone cleaning, and several re-chrystalizations.

swim didn't weigh , but the bio-assay was a-1; 2 people, 2 times.
swim was stunned by this, and feels that there must have been something in the post-rxn work-up that brought out the devil the first time; which swim didn't repeat on this crude effort of squeezing a line out of garbage.