Author Topic: *-Waterless A/B Questions-*  (Read 4438 times)

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kris_1108

  • Guest
*-Waterless A/B Questions-*
« on: June 05, 2004, 10:07:00 AM »
Hi

SwiK wants to dream about extracting atleast 5 boxes of 30(qty) 30gm Pseudo tabs. 1 box = 900mg pseudo (so 5 boxes = 4.5gms pseudo available.) At around $15/box, 'experimenting' with these is quite expensive.

Some type of waterless acid/base extraction will be used. With no pure Tetra around, the Tetra Trap cannot be used. Swik does not believe that these pills contain the new gakk, or that they are heavily gakked. They contain 500mg Paracetamol, which doesn't follow through the a/b, but upsets the amount of Sodium Carbonate required to base the pill mass.

Here are a few questions about the waterless a/b extraction. I think bees like Geez, Weaz, Shorty, Ware, Scottydog, etc may be able to help me.

1) The Paracetamol adds alot of weight to the pill mass. One box of these GUPS weighs about 20gms, however there is only 0.9gm of Pseudo. SwiK would add an equal 20gms of Sodium Carbonate per box. That means 100gms of Sodium Carbonate on a 5 box extraction! Is that ok?

2) Activating the base - Swik has the option of EtOH or dH2O. What are the benefits of each?

3) When using Sodium Carbonate (instead of NaOH) for basing, is it still a good idea to do a NaOH wash of the NP before titrating? (ofcourse the other hot/cold dH2O washed would be done...)



So far, the BARE procedure would be -

*2x Xylene boils
*Acetone boil
*Dry the PM
*Add equal weight of Sodium Carbonate (equal to the weight of the pill mass)
*Slowly add EtOH to form a paste
*Add Xylene to pull FB
*Gently heat/stir, decant Xylene
*Boil the EtOH out of the Xylene
*Wash the Xylene
*Titrate the Xylene
*Precipetate the Pseudo-HCl in Xylene for a final clean




former_chemist

  • Guest
Other indredients?
« Reply #1 on: June 05, 2004, 01:08:00 PM »
It would be helpful if you list other ingredients.
Can't you find some cheaper version? $15/box is outrageous.
Most of this has been covered at one time or another.

1)
Mol Wt. of primary adulterant=151.16
Mol Wt. of Sodium Carbonate=106
Since about half of your pill wt is the adulterant
you could use as little as 1/4 gm/gm pill wt.

2)
I would strongly suggest against H2O in a waterless extraction.  I always liked acetone but EtOH should work ok.  For a true waterless extraction use dry EtOH not 95%.

3)
Washing the Xylene with NaOH might be helpful with some
formulations that would otherwise cause problems.

kris_1108

  • Guest
Ratio
« Reply #2 on: June 06, 2004, 01:14:00 AM »
Thanks for your input, former_chemist.

I'm sorry I couldn't list the other ingredients. Here in Oz, they don't have to bee listed on the box  ::) . $AUD15/box is the average price here. The biggest amount of Pfed you can get in one box here is about 1.68gms, that's a packet of 7x240mgs. Some contain 1.8gms, but they are not packed with paracetamol or anything, and you need to give ID for purchace. Your name goes on a big central database. If you have been purchasing more than 1box/fortnight you are treated as suspicious.

Since about half of your pill wt is the adulterant, you could use as little as 1/4 gm/gm pill wt

It's actually about 95% of the weight is other shit. The other 5% is P-fed. I'm still not sure how much Sodium Carbonate to use.

wareami

  • Guest
Camp Pain....
« Reply #3 on: June 06, 2004, 01:38:00 AM »
Kris: UP until recently bees have been able to avoid the painreliever types. It's easy to see why they would choose to make them readily purchasable without jumping through hoops.
Geez is more familiar with the waterless a/b.
I'm thinking that since sodium carbonate is being used as the basing medium...75% WT of the pillmass should suffice.
I know it's still heaps of carbonate but if a certain pH isn't reached, the pfed won't budge.
And as former_chemist says....without a list of other inactives, it's difficult to say what might ride with the pfed and require further cleanup.
Good luck mate...




kris_1108

  • Guest
A Few More Questions...
« Reply #4 on: June 06, 2004, 12:43:00 PM »
How does a bee work out how much dH2O/EtOH needs to be added to activate the base? "A few tablespoons" probably wouldnt be enough for a 100gms of GUPS with 75gms of SodiCarb.

Also, what are the differences when activating the base with EtOH vs. dH2O?

former_chemist

  • Guest
only a little H2O
« Reply #5 on: June 06, 2004, 01:38:00 PM »
Only a little H2O is needed.  Too much risks activating nasties added to the pills that will trap your pseudo.  I am assuming the pills are a dry matrix formulation.  I would recommend against using H2O the whole purpose of this procedure is to add as little to the PM as possible to avoid activating the nasties.  Use acetone or dry EtOH.  With acetone you may need to add a few drops of water.  If you must use 95% EtOH (rather than dry EtOH) use as little as possible.  The amount used should be just enough to moisten the whole mass.

Shane_Warne

  • Guest
You might get about half a point of meth.
« Reply #6 on: June 06, 2004, 02:16:00 PM »
You might get about half a point of meth. But you probably won't get a single toasted sanger.

That isn't a 50% procedure you've outlined there, more like 30% at best. Though it looks nice on paper with more steps than a high rise building.

Ware, do you know if orange acetone dissolves pfed?

Because on the last clean a modified tetratrap was used, then, using a full A/B for the last pulls .
Upon evaporation there was an oil, that smelled really nice and took forever to evaporate, and smoked at a certain temperature.

It smelled nice he thinks because clove oil was used to wet a filter because he ccouldn't be bothered finding a more regular NP.

Anyway it came out nicely with dry acetone. But he doesn't know if it was the new oil gak people were talking about or orange mixed with peg or the clove oil.

The new oil doesn't smell nice does it?

Yields were bad btw, 2g out of 10.4, after about 7 pulls.

He added various garden salts in to the orange for the A/B pulls to try and force pfed out, it wasn't effective unfortunetly.

acetone rinses worked really well though to make a pristine outcome.

How does the Waterless A/B work with orange pills? cause the pfed didn't dissolve with the acetone rinses..and it might have been orange, he may have got lazy at the last minute while separating the layers. dont know.

12cheman12

  • Guest
swim has noticed one thing about orange, if...
« Reply #7 on: June 06, 2004, 03:14:00 PM »
swim has noticed one thing about orange, if basing with NaoH it gets activated, he belives it  gets activated because of the heat that NaoH produces, not the PH level. If Sodium Carbonate is used, less heat is created and orange is never seen, But as soon as heat is added to the pill mass sodium carbonate to help the freebase move to the NP... orange rears its ugly head. This made swim think that orange is activated by heat and not PH. Has anyone noticed this too?

Shane_Warne

  • Guest
yes, yes your right.
« Reply #8 on: June 06, 2004, 03:42:00 PM »
12cheman12, how are ya matey?

'If Sodium Carbonate is used, less heat is created and orange is never seen,'

Jesus, my little buddy, I think your right on the money.

But swim has been using heat because it states so in the tetra-trap. He didn't modify that part.

So does it work without heat?
My intuition would say it would basify just fine, but trust and habit let me down.

My little friend, I'm happy because you've just hit a glorious cover-drive in my books. For swim at least.

ChemNewbie

  • Guest
Tetra Trap
« Reply #9 on: June 06, 2004, 04:14:00 PM »

So does it work without heat?
My intuition would say it would basify just fine, but trust and habit let me down




If one doesn't employ heat with the tetra trap, he or she will wind up with little or nothing in the way of yields. Especially if Naptha is the NP used.




12cheman12

  • Guest
If xylene is used instead of naptha, then the...
« Reply #10 on: June 07, 2004, 04:16:00 AM »
If xylene is used instead of naptha, then the solvent does not need to be heated up.
Swim almost certain that heat is what activates the orange down here in Oz because, because there have been times when swim didnt use heat, no orange. And then when swims add heat to the SAME pill mass the orange pops up. Im sure just a lil experimenting will work this one out, Swim would do this himself but is not in the best situation at this current state in time. If anyone does have any findings on this make sure to post it ok guys, this could be a big help in the orange.

wareami

  • Guest
Orange....and now Yellow
« Reply #11 on: June 07, 2004, 05:54:00 AM »
>Ware, do you know if orange acetone dissolves pfed?
The orangeI and II were never known to increase pfed's solubility in acetone, but this newest yellow oil obviously does.
This yellow oil is hard to detect with the naked eye using alky extracts. But it does inhibit drying of the xtals and that is known fact.
So when yer shyte won't dry, you'll know why! ;)
It's soluble in every medium that pfed is soluble in.
The funny characteristic is the effect it has over pfed in the presence of acetone by allowing more than usual amounts of pfed dissolve in tone.
Pfed as we know is only very very slightly soluble in tone.
Same with meth.
But this yellow oil seems to interact with tone and changes the solubility somehow.
This oil does have a stench that isn't easily describable but you know it after you've run into it before.
This yellow oil is suspected to be Eudragit or of the Eudragit/Eupergit family of inactives.

One large area of concern discovered recently is that these compounds are listed as "Mutagens" and it's being determined now as to whether or not these substances are a health risk once they undergo the conditions of reduction from pfed to meth.
See

Post 498269

(wareami: "Eudragit", Stimulants)

I personally don't put anything past the pricks at this stage in their War on Drugs!
And based on some recent experiences, I'm certainly more inclined to believe today that they have no concern for anyone that may use these OTC's for anything other than their intended porpoise. FWIW


former_chemist

  • Guest
Health Risk
« Reply #12 on: June 07, 2004, 11:08:00 AM »
These compounds (Eudragit) are a health risk (mutagen) when used in the formulation as intended.  I can't see them being any less of a risk after a reaction.  Maybe someone should write a left wing (or right wing for that matter) journalist and tell them that the FDA is allowing mutagens to be used in OTC preparations.

The web site has interesting information on dissolving these compounds.  They can appearently be dissolved stepwise by a rising pH.  It would appearently be beneficial to dissolve the coating then extract.

I don't have access to a copy of the USP but there is a procedure in there that the pills with enteric coatings have to follow to be certified.  There is an acid step followed by a rising pH step.  The pill then has to dissolve in a certain amount of water over a certain amount of time.  I think there is agitation and some kind of membrane for testing as well but that may be for different formulations.

If someone with a copy can find that info it would probably be very useful to the extractomaniacs.

wareami

  • Guest
The Quick and The Deadly....
« Reply #13 on: June 07, 2004, 03:34:00 PM »
;D
Former: I'm pleased to see that you have returned and also have chimed in here on this.
These compounds (Eudragit) are a health risk (mutagen) when used in the formulation as intended.  I can't see them being any less of a risk after a reaction.
My greatest concerns have been that in order for these chems to have been approved by the FDA for inclusion may hinge on the fact that taken orally as intended, they may not activate and be delivered to the bloodstream but safely passed through the digestive tract and deposited as waste.
That is a best case scenario and an optimistic one I might add.
But as you suspect, I find it hard to believe that trace amounts wouldn't be left behind in unsuspecting consumers over time if used as intended.
Geezmeister had the foresight and concern to break the ice and post

Post 506882

(geezmeister: "Making myself sick", Stimulants)
after noticing some changes in the finished product and along with myself have noticed some ill after effects following bio-assay.
This might suggest that these ingredients, if not removed may undergo some chemical transformation in rxn that may pose as longterm health risks.
The "hangover" period seems to last well into 8 days after a 2day bioassay whereas before, 3days was needed to fully recover from a 7 day binge and it would be off to the races again.
This newest end result leaves one not interested whatever in repeating a run-in with this crap!
It's a real eye-opener of the unwanted kind.
So much so that it's taking all my willpower to keep from warning bees to stop getting product from this source.
However, until more scientific proof can be assessed and analysed I feel it would just cause widespread panic without having fact to back it up. As if they would listen to Ware....eh??? ;D
Anyway...Both Geez and myself are concerned...Ibee's doing some tests on the last gram of something he refuses to ingest because of the "2x4 to the head" effects it left after bioassaying 2grams of it in two days. A rediculously large amount compared to 1/2gram lasting through that period of time previously. 

1•They can appearently be dissolved stepwise by a rising pH.
2•It would appearently be beneficial to dissolve the coating then extract.

The problems I see here with both suggestions is:
1•In order to bring the pH up to the level needed to dissolve the coating, the pfed will travel with. The solubility characteristics of both are so alike under basic conditions that it's hard to separate the two.
2•Now this is the real tough one here.
Judging from all I've read to date, it appears they are taking individual components of the pills and coating them separately in order to insure contamination regardless of the extraction method.
At first I misinterpretted the patent to read that the coating comprising this gaak was an outer coating and maybe easily remved with the solvent used in it's manufacture.
Part of the work-around can be employed under that impression but it soon became evident that more was involved in order to completely remove it. In order to complete the work-around, it was necessary to study more about how they were including this substance.
This presented several problems that aren't easily remedied.
Squidippy sent an article a while back as a reference to what the pillfuckers are doing.
I feel it's posting will shed more light on this predicament bees currently find themselves in.
I will have to scour my refs to find the link that Squiddy sent, or maybe he can find it quicker and treat us to it....
But here is a similar ref to how they are using in Controlled-Release Diphenhydramine HCl Pellets Coated with Eudragit NE30D for an example.

Here is the PDF file of this document


...or you can view the HTML file here:

PharmSci

(http://www.aapspharmsci.org/view.asp?art=ps030214)


former_chemist

  • Guest
knowledge is a good weapon in the drug war
« Reply #14 on: June 07, 2004, 10:57:00 PM »
I can certainly see how some breakdown products of these polymers might be hazardous.  Methyl Acrylate monomer (methyl cyanide) was responsible for the bhopal disaster wasn't it?  The name of the monomer should be scary enough.  I think at this point everyone should be doing so sort of chromatography analysis on the extracted pfed and end product to determine the degree of contamination. TLC or even paper chromatography (does anyone other than lab students ever do that?), should be done.

There appear to be several classes of adulterants.  These may be mixed in a single formulation.

1) Coatings
  a) pH sensitive
  b) solvent sensitive
  c) heat sensitive

2) Binders
  a) pH sensitive
  b) solvent sensitive
  c) heat sensitive

3) reaction stoppers

The coating class should be fairly easy to remove.
The binding class is a whole different animal.
The reaction stoppers are supposedly targeted more toward anhydrous ammonia but the binding class may overlap.

At this point I think we really need to know how the pills are tested to verify bioavailability.  There must be at least one method of 100% extraction (possibly with some impurities).  This method would simulate digestion so it may take 6 (60mg), 12 (120mg), or even 24 (240 mg) hours. With this in mind 30mg tablets tend to look more appealing since they are designed to dissolve in 30 minutes (if I remember right).

Right now I am really wishing I had access to the USP to find the bioavailability test procedures for these things. If these things are designed to remain in the digestive tract we may have to resort to using osmotic membranes. Stock up on natural sausage casing now.

wareami

  • Guest
Squidippy's Plug...
« Reply #15 on: June 08, 2004, 06:55:00 AM »
Squiddy deserves the credit for the footwork on this one.

I feel it's posting will shed more light on this predicament bees currently find themselves in.
I will have to scour my refs to find the link that Squiddy sent, or maybe he can find it quicker and treat us to it....




Extended-Release Chlorpheniramine Maleate From Polymethacrylate Solid Dispersions by Supercritical Fluid Processing

(http://www.iirusa.com/drugdeliverypartnerships/index.cfm/Link=56)




Shane_Warne

  • Guest
Cheers
« Reply #16 on: June 08, 2004, 07:19:00 AM »
12cheman12,
'If xylene is used instead of naptha, then the solvent does not need to be heated up.'

That's agreed.

Your right about it beeing heat-activated, aswell.


Ware, thanks for the explanation.

Maybe it was a combination. he was amazed the tiny amount of clove oil just never went away, maybe the eudragit oil was keeping it there. dunno.

I thought that since this orange oilly, nice smelling stuff rinsed away in a few tone rinses, that it might bee a good basing medium.
But probably not, from what you said, it may not have been eudragit at all.

kris_1108

  • Guest
Water in the A/B
« Reply #17 on: June 14, 2004, 11:10:00 AM »
FORMER_CHEMIST, you said (re: activating the base...)

With acetone you may need to add a few drops of water.

I thought the base could be mobilised with dry acetone? Do you think traces of water will increase yields? What about some of the gakks that are active in the presence of water, therefor decreasing yields?

former_chemist

  • Guest
Experimentation
« Reply #18 on: June 14, 2004, 10:41:00 PM »
Various people have discovered through experimentation that a drop or two of water speeds up the basing process with minimal activation of the dry matrix.  This isn't always necessary if the reaction starts immediately then the acetone had sufficient moisture to catalyze the reaction. It does seem to increase yeilds in some cases.  Of course as new formulations come out this method may no longer be applicable.

Jacked

  • Guest
Reply on naphtha and heat
« Reply #19 on: June 15, 2004, 07:17:00 AM »
Heating naphtha helps freebase meth (oil) dissolve in it but if used cold the base still moves through the naphtha, it resides on top of the naphtha if cold.. Pseudo freebase moving into a non polar is in a solid form anyway and will push its way into the layer even using cold naphtha (cold being room temp.
 I would think heat would be necessary for bicarb to baseify pseudo in the first place wouldn't it?.