Author Topic: Precursors for Ozzies (RP/I2/E)  (Read 21563 times)

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the_happy_chef

  • Guest
losing eph/meth
« Reply #60 on: January 07, 2004, 01:52:00 PM »
it's only going to get washed out with the water if:

- there's not enough solvent to dissolve all the freebase so some of it is trapped and can't move into the solvent

- u didn't base it enough, needs to be at least ph 12. or just lock the fucker, doesn't make any difference

- u separated when the two fractions were emulsified. now that was a dumb idea wasn't it?

:)

spectralshift

  • Guest
2) Are you suggesting to use HDPE tubing for...
« Reply #61 on: January 09, 2004, 09:59:00 PM »
2) Are you suggesting to use HDPE tubing for these distillations? (Sorry, kinda confused from your last post, you mention tubing, but then seem to call it HDPE, just verifying)

High-Density polyethylene. Black irrigation tubing.

3)You mentioned earlier somewhere that the ste extraction would not work on practially any aussie pill. Does this mean that aussie pills are even harder to extract than US pills?

It's just not a thorough clean at all imo man. A xylene boil, a boil in the VM&P out of VideoEditors pantry will achieve identical results as far as I can see. As a clean I think doing the boils separately is actually better.
When the solvent used is saturated it precipitates any further gak, and that's it.

This is how that clean works, simultaneously: the pfed is extracted in to the isopronal, gak is dissolved in the two solvents, xylene and naphtha...as the temperature rises, the isopropanol is boiled off and the pfed precipitates..the gak remains solvated in the naptha/xylene.

But here's what this description doesn't discribe: In the first instance: No where near all gak is solvated, it just doesn't happen in these times, so what the solvents don't dissolve, they precipitate obviously.
(Whether it be that the solvents are saturated with gak, or if the solvents just don't dissolove a particular gak)

In the second and final phase of boiling, the propanol has evaporated, the pfed is precipitated, along with any gak which has been solvated.

About Auzpills, here is what makes our task more difficult (blessing in disguise), we don't have innactives listed on boxes, they are more expensive, we have less brand options, less pills per box. The main problem is that Auzbees can't run as many tests because of all those factors.



Swim has often wondered why no one has succesfully used dilute acid/base soaks and stuff. Some say that this activates gakks, but surely there is a way of getting a gakk away from the sudo, we just haven't found it yet

The reason for this is undeniably beecause Geezmeister & Wareami have taught generations of newbee's to stay well away from water.
You'll now in the coming monthes see this methodology kast aside IMO. Well I know it will... ;D

In fact it's already started, look up a post by hellman recently (there will only be a few), ballzofsteel describes a boil with a splash of vinegar a bit in to the thread to remove cellulose.

Swim has been following, with great interest he might add, your posts in the tetra trap (and others) thread. You have made some interesting points lately. Swim is curious to know what you would call the "ultimate/universal" extraction procedure (ie what do you use). Obviously you may wish to keep this secret, and swim totally understands if you do.

lol Nah it's cool man, I don't really have an ultimate clean, up until now I thought we were working together for an ultimate clean. But competition is good, it dosn't lend itself to openness of ideas though.
My current thinking is that dry basing is the way to go, as it will always get some results, tetra or no tetra, no bottom solvent either.
Problems that affect this fundemental plan from being quantitative (100%) are theoretically glues and plastics, they stop all the pfed molecules from based, and also successfully based pfed molecules from being released in to the NP, cellulose and hydrogels have the same net effect here.
So these problems must bee solved in pre-washes, before we enter our feedstock in to the dry basing phase we've agreed is the second step.
To do this in a virtually lossless manner we do this.
Place the ground up pills in 3 coffee filters, place a binder clip over the lips to close it, we tie a piece of string to the clip-ring and dangle it in our boiling solvents.
Ill continue... To restore a nice chalky texture to the pill mass in the coffee filters to restore something which is easily ground with the base, we pestle ourselves up a piece of chalk and add it to the washed pfed. (Please note: Chalkyness won't obstruct basification as glues and plastics will.)
Solvent selection for this de-plasticizing, de-glueing and de-cellulosing phase.
1. A 12hr soak in acetone to dissolve out celluloses. (Uncertain whether a boil should follow this, it will dissolve some pfed, it's a matter of whether that is a price necessary to make de-plasticising/de-resinating  gains)
2. DCM, Perchloroethylene. I'm not certain if DCM is a subset of PCE or if they don't quite overlap. Either of these will remove anti-histamines as a bonus, but plastics and glues are the concern.
3. Toluene and or xylene to remove waxes and glues.
Final Preparation for Dry Basing
A nice dry, chalky texture is the sole pre-requisite for this. In order that the feedstock can be mixed with the base.
If it's discovered that the result of our teabag washes is a load of gooey plasticky shift (still), we must decide, more washes? Or force a chalky texture with the addition of chalk or similar?
We do as much mixing in the filter papers as possible, both of the base with the washed pills, and of the chalk with the pills if this is needed.
Dry BasingThe Main Show
It seems a simple enough concept, and it is, except for orange, *sad*.
Now let's consider orange...It's a little cunt that tranforms in to an orange oil when a) too much base is present, i.e the pH is too high. And b) when a proper amount of base is added and heat is applied.

What this orange fluid does is this: It dissolves formed freebase – so that instead of moving up in to a Non-polar as they usually would, they remain dissolved in the orange oil alternative.

I dare suggest that if you left it in this state for a week, a good proportion would cross the interface. i.e out of the acqueous orange and in to the NP/oranic phase. (But we want to hurry things along a little dont we?)


Note this: If the critical pHis first reached to achieve a proper basing i.e fb has opportunity to transfer to a NP without orange hindrence...but then it's accidently overstepped to Orange water release, then the TIME and OPPORTUNITY between these two points is of great importance.

- So to give ourselves the best opportunity of the TIME being a long time between these two points slow basification should bee used.

- To give the pfed the best OPPORTUNITY to use this time. i.e to escape in to a Non-Polar before the orange pH is accidently reached, we must give the based fb the greatest interface surface area
through which to escape.

With a bottom-layer of a chlorinated solvent, and a top layer of a less dense solvent such as toluene or xylene, we provide twice the interface surface area.

But then at the critical point when the orange water has been released and has the remainder of the pfed which didn't make it across dissolved in it these are the new enemies to complete phase transfer of the pfed.
i)Viscosity of the orange/fb/water solution. As this quantity/variable increases, so does the following quantity;
ii) Time required to finish off phase transfer of fb to NP.

So what do we do? Oh no! sad - We've already got twice the interface surface area, isn't that enough Jesus? Dad? No Son, that just isn't fucken good enough – you fail you fucken losty!you embaressing little barstad
We use warmth and a generous amount of time, depending on how well it goes.
We use acetone in the basing medium to decrease viscosity.
We use acetone in the basing medium to bee partly miscible with the DCM/ toluene or xylene
We use alcohol for it's limited miscibility with DCM and toluene.
In combination these weaken the intermolecular forces between the fb and the orange, and also keep the orange strapped for water that it needs to work to it's full fb hugging ability.


We're getting some pretty cool test results coming in from the TetraTrap thread, 1 from geesemaster, 1 from SAWTY both testing alcohol...and a stranger has posted a result using acetone. Note that these results are only of importance in selection of a basing medium.

Anyway Ill stop thare for now. Tell me if you need clarification/simplification.

suss

  • Guest
Thanx spec
« Reply #62 on: January 10, 2004, 04:04:00 AM »
Thanx spec. Nice post. Agrees with everything I have come to think, which is basically that if you use a nasty solvent, with heat and time, you can do good! Interesting that you suggest adding chalk to improve the texture. Swim feels that this approach of "attacking" or beating the gakks at their own game is better than current ideologies, where we try to avoid them and fear their presence.

BTW:

1) you mention that the DCM etc will kill antihistamines, does it work with fexofenadine HCl, commonly found in "telslow" pills?

2) Given the easy availability of DCM, do you think it is really worth the extra trouble to get tetra? Seems we could be a bit more liberal with DCM, and give the pills a real long soak with excess solvent, and even a good boil.

Had alot of questions for you lately, but will soon have some results from swim's conceived "Dichlorinated MEKanic" extraction, which promises to work wonders with aussie pills full of paracetamol :)

Cheers mate.

wareami

  • Guest
Mr. Spectral sir...
« Reply #63 on: January 10, 2004, 04:04:00 AM »

lol Nah it's cool man, I don't really have an ultimate clean, up until now I thought we were working together for an ultimate clean. But competition is good, it dosn't lend itself to openness of ideas though.




Excuse me mr.spectral but you really need to get your head out of your ass and get some fresh air and quit poluting the board with this nonsense!
You are starting to offend me and in no way shape or form will you ever get any support from this corner if you do that!
Just a word from the wise.
You made several misinforming remarks in your last reply regarding Geezmeister and myself.
Straight out water extractions don't work period on any pill.
Nobody said that water can't assist after drymatrix and other gels are dealt with. The IDEA proves this. ie...70%isopropyl and denatured alky.
A/B's are done successfully everyday using Straight2b butit doesn't deal with OII gaak. But mainly on pills not comprised of drymatrix.
The latest finding in the tetra trap utilize water.
What you stated in it's intent was false and misleading!
If you continue this crusade like your the lone stranger...I assure you, you will be!
Tighten UP!




spectralshift

  • Guest
Alrighty
« Reply #64 on: January 10, 2004, 10:55:00 AM »
1) you mention that the DCM etc will kill antihistamines, does it work with fexofenadine HCl, commonly found in "telslow" pills?

I don't think it will man no,(I don't have the properties for the hydrochloride) however the basification step will! Here's the properties for the FREEBASE

'Properties:  Crystals from methanol-butanone, mp 195-197degrees (Carr) ; also reported as white crystals from methanol, mp 142degrees-143degrees (Kawai)'

Most of it will precipitate out if it isn't wanted by the basing medium, because the NP won't want it.

2) tetra's a super solvent, so I'd use it if it was on hand, but as far as the DCM goes, yeah bee liberal, it works real good.  8)
Hot tap water will boil it! It's non-flammable. 10 boils can bee done in 20min...

and so to you my ambitious newbee buddy.  ;)

I'm going to read over your extraction again OK? remember that a basification step will do the job for paracetamol.

suss

  • Guest
DCM
« Reply #65 on: January 10, 2004, 09:24:00 PM »
Spec,

Just read that DCM and alcohol form azeotropes. 2 questions:

1. I guess the DCM is dry enough to use as is, one distilled out of the paint stripper. Is this correct, or should I dry it further with Mg sulfate?

2. What about the alcohol? How should it be removed? Can you just wash the paint stripper with water before distilling, or will the alcohol prefer to stay locked in the DCM azeotrope?

Swim has come up with what he believes will be a killer extraction, using some techniques that he hasn't found discussed on the hive. Will try soon. You're gonna love it. Doesn't use anything new, just some different solvents and different ways of soaking/washing. Will use minimal solvents too. 

BTW, do you know if the black HDPE tubing is attacked by DCM, Acetone or MEK.

Cheers

pyroflatus

  • Guest
DCM from paint stripper
« Reply #66 on: January 10, 2004, 10:12:00 PM »
1. I guess the DCM is dry enough to use as is, one distilled out of the paint stripper. Is this correct, or should I dry it further with Mg sulfate?
First you should wash the distilled DCM with conc. H2SO4 then 2x with H2O, then dry with MgSO4.

2. What about the alcohol? How should it be removed? Can you just wash the paint stripper with water before distilling, or will the alcohol prefer to stay locked in the DCM azeotrope?
The water in the previous suggestion will strip any ethanol (presuming there is any) from the DCM. Whether you need to  dry the DCM depends on whether the synthetic route you've chosen requires dry DCM.

HDPE solvent compatibility

kimble notes

(http://www.kimble-kontes.com/pdfs/solvent_compatibility_2.pdf) lists the following compatibility for HDPE:
Acetone : moderate effect, fair
DCM: moderate effect, fair
toluene: minor effect, good
Searches for "solvent compatibility HDPE" on google will yield results.

more notes

(http://www.millipore.com/catalogue.nsf/docs/C7873)

placebo

  • Guest
Re: You are starting to offend me and in no...
« Reply #67 on: January 11, 2004, 12:31:00 AM »

You are starting to offend me and in no way shape or form will you ever get any support from this corner if you do that!



Gee, scary threats!

On a seperate note, your all getting way too complicated, as much as I hate to sound like hellman. Unless of course US pills are suddenly heaps harder to extract then Aussie pills, though I doubt it.

An A/B will rid you of paracetamol.




hoffman

  • Guest
sounding like hellman?
« Reply #68 on: January 30, 2004, 06:13:00 PM »

jemma_jamerson

  • Guest
placebo
« Reply #69 on: January 30, 2004, 07:59:00 PM »
are you serious, no dry acetone boils, are you suggesting that i get any ozy 'sudo' pack with 500 grms of para in it and simply a/b the bastard and it will rid you of the paracetamol?

sounds too good to be true

btw have you ever tryed to a/b the pills that are 'sudo' 'f_d
wasent a pretty site..

ow and shit mate, swim found a pill brand that is sudo sulfate with an anti hist in it, the only 120 milg left on the shelves in swims area.

would doing an

a/b -> dry acetone boil? to convert to hcl then rid the anti hist?


sublevel

  • Guest
aussie pills
« Reply #70 on: January 30, 2004, 08:29:00 PM »
Dry basing the cleaned pill mass works wonders over here especially on 120mg variety(telslow).This is how swis swims with these brown and white bricks.

mortor & pestle pills finely add to pyrex

add xylene (1-2" above pm) boil whilst stirring
2mins,settle, decant, discard (total of three times)

dry pm, pm should be fine chalky , mortor & pestle sodium carbonate and sodium hydroxide (equal carbonate, 1/4 hydroxide compared with pill mass)pm1/carb1/hydr.025

mix into pm then add c*c b*ak**en by spraying into can lid
and pouring and mixing into base/pill mass, until it looks like fine crushed farex with no free running fluid.

add xylene heat slightly stir 1-2mins decant thru single filter(total of three times)wash with hot dh20, wash with cool dh20 twice.

freebase in non polar usually gas to get hcl form.
yeild is 80-90% of very clean product.

br*k**en here does not contain tetra but the following

methylene chloride           75-09-2 (cas)           10-30%
chlorinated hydrocarbon      127-18-4(cas)           30-60%
petroleum distillate          no cas                 30-60%
liquified petroleum gas     68476-85-7(cas)          10-30%

any ideas on why it works so well?  swis has experimented with all the range of c*c aerosols with said product to work best by far. tried isoprop, tone, methylated, to motivate base, yeilds were much lower and not as clean.

anyone else use similar methods?

the aus pills are all very different here from one brand to the next just like our solvents compared with the USA. dont know if there is a universal cure but with dry basing expect to get results, just the workup is slightly different with different brands prior to basing.

SHORTY

  • Guest
I use a similar method
« Reply #71 on: January 30, 2004, 10:44:00 PM »
Except for the initial xylene washes as well as the water washes.  I use a electronic cleaner spray but i don't know whatis in it cause its not listed it just says non-toxic.  No company name either.

Heres how i do it:

1.  Weigh pills and put in blender along with an equal amount of sodium carbonate and blend until fine powder.

2.  Pour powder into a beaker and add electronic spray until the powder is saturated and stir thoroughly.

3.  Add xylene to cover the pm by about 2 inches and add a few mls of dh2O while stirring with a glass rod or bamboo chopstick.

4.  Place beaker in microwave and bring to a boil and remove and stir and allow to settle.

5.  Decant xylene into a clean beaker through a filter and repeat 3 or 4 times.

6.  Gas the xylene to get hcl and pour through a filter and repeat until no more precipitates when gassed.

7.  Take the gassed xylene and put it in a visionware saucepan and then add methanol to the filter containing the pseudo to dissolve it and add this to the saucepan and rinse the beaker with methanol and add to saucepan.

8.  Place a thermometer in the saucepan and place on hotplate.  At 65C the solution will begin to boil.  Continue to boil until the temp reaches 105C and remove from heat and allow to settle for about 1 minute.

9.  Decant the hot xylene and the pseudo should stay in the bottom of the saucepan.

10.  Flood the saucepan with acetone which will begin to boil due to the heat of the saucepan.  Stir the acetone and then decant and repeat.

11.  Allow to dry and your done.

This is the fastest, cleanest, route to pseudo that i have found so far.  I have done it this way for the last few months and it works great for the pills in my area.  I just did a batch of 333 white, 60mg w/trip and got back 17.88g of super clean pseudo.


sublevel

  • Guest
base amount
« Reply #72 on: January 30, 2004, 11:45:00 PM »
swis used to add carbonate only equal to mass and found that adding extra hydroxide increased yeild.(without burning pill mass)

swis tried basing without xylene washes, but xylene pulls needed much rinsing. yeilds were not much dif.  Found it better to rid mass of xylene soluble junk first then base.

the psudo/methanol/xylene  sounds good, will try to substitute methylated spirits for methanol.

after gassing xylene swis filters, drys, mek rinse.add dh20 then evap. very clean 80-90%. sometimes will wash water with hot xylene.

intrested to know whats in your can. any numbers on it?

suss

  • Guest
Sublevel
« Reply #73 on: January 31, 2004, 01:26:00 AM »
Sublevel,

The reason your canned stuff works so well is the methylene chloride, also known as dichloromethane. A very good solvent used in paint stripper. Also the chlorinated hydrocarbon. Can't be bothered to check the CAS, but it might be tetra, which we all know and love. Simple.

Master_Alchemist

  • Guest
Tetrachloroethylene
« Reply #74 on: January 31, 2004, 02:01:00 AM »
Shorty, the active ingredient in your electrical cleaner, is most likely Tetrachloroethylene(TCE).
Stick with it mate, your onto a good thing; Works wonders removing povidone and polyethylene glycol, not to mention anti-hystamines ;)
For the record, FUCK RP/I2/E...old school, old problems, new chem watching strategies :(
Also, wtf/who is swim & swix?? You guys are confusing the fuck out of me!

sublevel

  • Guest
cheers
« Reply #75 on: January 31, 2004, 04:06:00 AM »

12cheman12

  • Guest
because paracetamol is failry insoluble in...
« Reply #76 on: May 12, 2004, 11:39:00 PM »
because paracetamol is failry insoluble in cold water, if one dissolved his pill mass in water then brought it to near freezing temperature in a freezer should most of the para drop out? and what effects would the near freezing temperatures have on the pseudo?

kris_1108

  • Guest
Para- SHIT-amole
« Reply #77 on: May 13, 2004, 01:44:00 AM »
In my experience, the paracetamol 'crystalises out' as the water temp approaches 0°c. Only 1.4gms of para will disolve in 100mLs COLD water.

However, DONT add water first! Atleast do some solvent boils and pull the pseudo/para with alcohol, and then deal with your pfed/para.

Let me know how you go.

ning

  • Guest
AFAIK, since paracetamol is a phenol, simply...
« Reply #78 on: May 13, 2004, 08:07:00 AM »
AFAIK, since paracetamol is a phenol, simply performing an acid-base extraction will remove it. It will for a water-soluble salt with strong base.


grokstar

  • Guest
MEK sucks your yield
« Reply #79 on: May 21, 2004, 05:44:00 PM »
I`ve found hot MEK dissolves much more of what you want than is really acceptable,  Its stricken from the extr proc.

And for the benefit of Master_Alchemist (chuckle) above -
S W I  - someone who is.

I was never here