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why iso..??

Started by UncleFester, August 09, 2004, 11:21:00 PM

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Ascension

If denat could be purified by simple distillation then it wouldnt be a very effective denat would it. People would just distill it then drink.
The denats have practically the same BP as the ethanol making it impossible to purify this way, infact its almost impossible to purify denat alcohol anyway from what i know.


UncleFester

I wrongfully posted that the results from straight iso-OH followed by KOH boil of gas station 200 mg guifenesin/25 mg ephedrine was suitable for further use. It is suitable for shit. These pills need a pre-soak to clear the inactives. I will report back later on details.

UncleFester

the superficial commentaries come in, consider that I have been extracting these ephedrine pills for about 15 years throughout their various transformations. I'm not a newbee. When the 100 mg. guifenesin pills came out, one could extract by first soaking in toluene. When the 200 mg. guifenesin pills came out, a toluene pre-soak, then base with NaOH in akly, then extract with naptha worked just fine. The last couple of years that one worked poorer and poorer as more shit went into the pills....ephedrine pills have always lead on formulations to market.
Now this failure on the KOH method. It may well be that the 200mg and associated shit just has to have a pre-soak. The alternative is that this is a new breed of pills. Time will tell.

BOS

About these methacrylic polymers,is there solubility not dependant on ph?
Like,dont they become insoluble at around ph5?
Why not extract with alcohol,filter,acidify alcohol pull @ph5,wait,filter and then carry on with what ever extraction steps you feel are still needed.
Sorry if this has been mentioned.

Some reading for you Ware :)

http://www.pharmcast.com/PatentToSubWeb/Classification/Classification500.htm#Microencapsulation



like you havent read it all already.

UncleFester

Let's just ignore the difficulty in judging the pH of an alcohol solution, especially at a near neutral pH like 5, and suppose that one of the polymers in the pill mix, eudragit, has a solubility minimum at pH 5. There are still al the other polymer additives, and they are chosen so that they will make no end of problems. Things like polyethylene glycol(PEG), that yet inidentified filter plugging material, and on and on. All the new additives are polymers. By breaking them first, one has a much clearer field...one the people who thought up the additives hadn't covered. You may not end up with a pristine product just by alky extraction and KOH boil, but it at least gets you to a product that works. The product then can also be freed of residual crap by recrystallization. pH tweeking of the extracts has been tried, but other additves get through. It's best to clear the field, then work.

metalgirl

here's a miseable tale just to add to the colourfullness of this thread....tried a caustic alky reflux on about half a cup of ground pills and ended up with about three cups of black shit that had the ability to soak up endless amounts of toluene...a whole litre of tolly was exhausted...the tiny amount that could be poured off was evaped to reveal half a teaspoon of brown crud from a potential of five grams sudo....misery ensued and some ephedra was purchased....

tina_craig

Every KOH boil swim has performed has left him happy with at least 50% of initial gear. Getting a 10mg ready.


UncleFester

would caustic be NaOH? That is the usual terminology...

metalgirl

yes, naoh...i guess i was avoiding the whole koh vs naoh subject since it was recomended not to use naoh...i thought it wouldn't matter too much since it works wonders on an ephedra extract but something tells me your going to tell me different....i did reflux it for an hour....what do you reckon?

geezmeister

Yes, it matters. KOH and NaOH have important differences here-- KOH is more readily soluble in alcohol than NaOH. You want that water in the alcohol...you cannot succeed without it.


Ascension

NaOH is also know as caustic soda and sodium carbonate is soda ash, not to sure what potassium hydroxide is referred to as but.


nuke

(Waste of time)

Edit:  Depending on where you live, you might be able to distill it or not...  If you're in the EU:

Post 511332

(methyl_ethyl: "EU Ethanol Denaturation", Stimulants)

Jacked

potassium hydroxide is referred to as pot ash I believe.
 Metalgirl, What happened to the alcohol? did you separate it from the mess in the bottom of the beaker before evaping it? Brown stuff sounds burnt to me...
 Separating the alcohol and evaping will yield at least 50% in a freebase form if KOH was employed. A DH2O wash of the freebase and titrating back to an HCl should be clean enough for use. You could add toluene and gas if you don't like titrating.. Swim says use the freebase anyway. It makes things simple.. Toluene can be added to the snot left in the beaker to pull for higher yield. process this separately..


tina_craig

315 24 x 30's boiled in 450mL 91% ISO IPA 15 grams KOH added at boiling point, boiled 30 minutes.  Top layer decanted off of oily layer on bottom and evapped to near dry, flashed with tone (stupid part?) and filtered.  Covered with 100 mL tolly washed twice with dh20, separated and gassed tolly, became cloudy and white material settled on bottom but material passed through filters.  Entrained water assumed.  Evapping tolly extracts and will cover with tolly again and allow to sit to drain entrained water and regas. Does this sound right?


metalgirl

Damn I've had a bad few days...two posts rated as misinforming for reasons which are quite obvious and now this....I'm afraid I've really led us up the garden path, through the fields and over the mountains here....
       I did this proccedure many months ago and whilst posting about it my recall of the event was shocking....In fact I had allready worked out what was most likely the problem...this is embarrasing...you see, the great god of slackness had guided me that day to not worry about ridding the pills of paracetamol just to see what would happen....well it all swelled up and went pitch black so I guess that's what happens...though, interestingly the proccedure was performed on an alky pull, not the raw pill mass which makes the amount of black shit I got quite remarkable....oh, and Jacked; it was refluxed in an oil bath at 100 C so it wasn't burnt by heating..
     Also, though I have a strong inclination toward believing you guys about koh vs naoh (since I know squat) I can't help but wonder how important the difference is since the naoh/meoh has proven to be very effective on an ephedra extract.....no emulsions in work up..I guess this is very different to pills so the difference may be vital in pill hacking...
       Uncle Fester, what's this about water?...I've been away from the hive for months and months...better read the whole thread....god! these must be the most useless posts I've ever made..

UncleFester

This subject was covered in detail in the thread along with experimental, you'll find it with some looking. Also, the old term for KOH is caustic potash.

metalgirl

Just out of interest, i've just been reading about biodeisel....which is made by reacting vegetable oil with koh or naoh in methanol. The article i read says naoh+methanol= sodium methoxide. Here's a bit of the article.....(this may all be irrelivant so i don't mind if you down rate this)
           

               "TRANSESTERIFICATION"

In transesterification, lye and methanol are mixed to create sodium methoxide (Na+ CH3O-). When mixed in with the WVO this strong polar-bonded chemical breaks the transfatty acid into glycerine and also ester chains (biodiesel), along with some soap if you're not careful (more on that later). The esters become methyl esters. They would be ethyl esters if reacted with booze (ethanol) instead of methanol.


oh yeah, here's a definition of caustic:

Capable of burning, corroding, dissolving, or eating away by chemical action.
Corrosive and bitingly trenchant; cutting. See Synonyms at sarcastic.
Causing a burning or stinging sensation, as from intense emotion: "Most of all, there is caustic shame for my own stupidity" (Scott Turow).

n.
A caustic material or substance.
A hydroxide of a light metal.
The enveloping surface formed by light rays reflecting or refracting from a curved surface, especially one with spherical aberration.

tina_craig

swit_c just finished another KOH boil, 3.60 grams available.  175ml 91% ISO IPA used to extract, then right at boiling 5 grams of KOH chips were added and boiled 30 minutes.  At 20 minutes of boiling 1 more gram of KOH chips were added.  This was then allowed to cool and the bottom layer which was just as swiuf described it except a little more yellow was separated off through a sep. funnel.  ISOIPA was then evaporated to give a large amount of crystalline pseudo.  To this 20ml dh2o added then, this was poured into sep. funnel then 75ml of toluene was added to evap. dish and used to get up all the xstals and moved to sep. funnel. Then 1/2 of total volume of tolly was added in dh2o 3 times.  Now the tolly is sitting to drain entrained water.  Question is should the tolly look like milk right now?  Is this a shitload of entrained water or is something wrong?


Scottydog

Swim doesn't trust this "let the NP sit shit" to remove entrained water. SetUP a funnel in a mason jar. Add a piece of cotton ball to plug the funnel and dump in about 60 grams of dry MgSO4 into the funnel.

Then pour your NP layer through the epsoms and cotton. Once it is done dripping into the mason jar, then you can GO ahead and gas it! Not drying your NP will rob you of precious precursor. I know Fester recommends the sit and wait in his writeUP but Swim would advise against it. It will work occasionally but once you've suffered the mystery of the disappearing pseudo, just one time, its enough to make you want to do things correctly and not take shortcuts. If the milky consistency is something other then moisture, the filtering may go a long way in dealing with some of this.  ;)


tina_craig

kewl, thx sd, and by dry you mean baked in oven at 400 degrees for 1 hour?