Author Topic: why iso..??  (Read 16316 times)

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abominator

  • Guest
That's what he means, to bake the epsom salts...
« Reply #40 on: October 04, 2004, 10:10:00 PM »
That's what he means, to bake the epsom salts til dry.


tina_craig

  • Guest
These pills suck! Tolly sat all day and ...
« Reply #41 on: October 05, 2004, 02:54:00 AM »
These pills suck! Tolly sat all day and cleared, gassed and white formed but falls right through filters.  Evapping all tolly now.  Had the same problem when used these before and got triple gaaked in rxn.  These were left overs and swim will NOT be pursuing this mix again.  Don't even know if evaps will be safe to use.


UncleFester

  • Guest
milky toluene
« Reply #42 on: October 05, 2004, 12:48:00 PM »
What was the ID of these pills? It's an important bit of info so that new formulations can be tracked. I think you were a bit on the light side with the use of KOH, also, the wash with water of the toluene extract was skipped. Much shit comes out on that wash. Once most shit has been removed, the toluene will generally shed any water upon sitting a couple hours and be fit for gassing once transferred to a clean beaker.

tina_craig

  • Guest
Uncle: These were the inactives: Ammonium...
« Reply #43 on: October 05, 2004, 06:23:00 PM »
Uncle:
These were the inactives:
Ammonium Hydroxide, carnauba wax, croscarmellose sodium, dibutyl sebacate, thylcellulose, FD&C red #40 Al. Lake, FD&C yellow #6 Al. Lake, fumed silica, hypremellose, lactose, microcrystalline cellulose, oleic acid, polyethylene glycol, povidone, pregelatinized starch, silicon dioxide, stearic acid, sucrose, talc, and titanium oxide.

$1 24 x 30

Tolly was washed 3x with 1/2 volumes of dh20.

This is second try at this particular super generic brand.  Same story last time. Tolly was evapped to give back 2g out of 3.6 possible of soft, flaky, slightly sparkly FB pseudo.

These were so generic it actually stated on the box that they were not produced by the same manufacturers of Sudafed.  Don't want to names sources though.  Will publish as much info off of box as possible when swim gets home tonight.


tina_craig

  • Guest
More on the monster pseudos: What info is...
« Reply #44 on: October 06, 2004, 02:55:00 AM »
More on the monster pseudos:
What info is swiuf looking for, a lot #? swim doesn't want to list anything that shouldn't be listed.

Pharmacist's Signature
Lot#: ZS4E078 H
Pharmaceutical Formulations, Inc.

Swim hopes this isn't too much info or considered naming sources, just wanted to make sure swiuf got all the info needed.  If too much was listed pls let swit_c know what can be posted from this list and future posts will be less listed.

BTW, washed tolly evaps 2 grams original with tone to give 1.5 grams of pseudo.  Dissolved in methanol and in process of rxtalizing.  More later.


UncleFester

  • Guest
6 gr KOH?
« Reply #45 on: October 06, 2004, 04:47:00 AM »
I missed the repeated water washes in your procedure. In any case, 6 or 7 gr of KOH was enough for the Walgreens generics which were closely in accord with the original patent. When moving on to the brand names and Wally Worlds store brand, the KOH had to go up to 10 gr per 100 30 mg pill. If the toluene extract is cloudy after water washing, and won't settle out...that is uncleaved polymer dragged through. Up the KOH level, and let us know what happens. You may also have to filter the toluene extract, but in my experience that was only needed when using makeshift KOH from NaOH and KCl. Boost it up, and let us know.

tina_craig

  • Guest
Tolly did finally clear and was gassed to no...
« Reply #46 on: October 06, 2004, 05:29:00 AM »
Tolly did finally clear and was gassed to no avail.  Evapped the tolly extracts for the FB.  Washed with acetone, dissolved in methanol and is slowly recrystallizing with the nice cool night.  Swim has 3 or 4 more boxes of these and will up the KOH to ratios given.  Any other tips or pointers swiuf?


wareami

  • Guest
Just some thoughts!
« Reply #47 on: October 06, 2004, 05:29:00 PM »
Uncle Fester: This condition being described with filtration problems and milkiness is reminiscent of hydropropylmethylcellullose and MCC in combo that comprise the DryMatrixFormulation(DMF).
That DMF still runs rampant in most all the pills described in this thread and in most reports lately that list inactives...
Unc_F, Being the gaak thwarter and inventor of this technique that sidesteps eudragit, also recently discovered and shared the unique mindset of getting the gaak out of the way first then dealing with the goodz for further purification.
I wouldn't put forth this recomendation if it could feasibly interfere with method or instigate extraction problems.
So with that U_F...Ibee wants to suggest to you first a method that may help sidestep the problems others are reporting.
A pre-extract Tetrachloroethylene wash might work wonders on the pillmass at removing some of the nasties that are forcing higher KOH amounts to be used in order to skirt by all the cleavage in that beautypageant ;D
Just a suggestion and a thought...nothing more!
If it helps...it helps...
I strongly doubt it could hurt.
Happy extracting!


UncleFester

  • Guest
pill ID
« Reply #48 on: October 06, 2004, 11:56:00 PM »
Not knowing the pills ID has slowed up my reply, however, if they are the Wally World pills, or brand name, when enough KOH is in the mix, it makes a milky solution upon hydrolysis, and the milkiness consists of white flakes. They settle out over a few hours, and workup proceeds as usual. This variety takes a larger load of KOH. I can't understand the squeemishness about mentioning pill brands. No mention of sources is meant to prevent some innocent supplier of useful chems from having his life turned into a living hell. It's not meant to prevent ID of an OTC product sold by the millions. I barely have time to get my dishes done, so directness is invaluable for me. I doubt it is a dry matrix formulation. More likely that gak exhausted the KOH...I could be proven wrong...

wareami

  • Guest
Specifics...
« Reply #49 on: October 07, 2004, 12:56:00 AM »
On sourcing and specifics, I won't go into the thick of it.
And I agree that it wouldn't hurt the source much nor would it likely have an effect on what they are doing with newer formulations.
I do feel that one's livelyhood and liberty could be placed in jeopardy if they include so much information that is undeniable in the court of law that this is no longer a hypothetical theory based discussion.
Lot#'s...exp dates...NIC numbers...all that info adds up.
Description, smells, etc... of certain gaaks might even narrow down ones illicit activity.
Even if it were allowed and the Hive could never be held accountable today...doesn't mean that won't change tomorrow.
There is a fine line being walked as it is in regards to the sites disclaimer and the freedom we are given to speak our minds.
I wopuld rather side with caution to insure the site's longevity and safety if in fact anything was ever challenged here.
That's just my opinion.
There is a distinct odor of eudragit and our friend chemosabe brought this up while not being able to put a finger on it. I'm happy for that...for him/her/it that shy away from such identifying info.
While I know for for a fact the name of that aroma...I'll not disclose that in writing.
I'm looking at it like this.
They know who Ibee is...they know ibee's name...
They can only guess what Ibee's doing based on what he tells them he['s doing...and he's so full of crypticBS you'd have to bee a fool to take his word for anything!
So to tie UP the loose ends for them....Well Fuck that!
Ibee'll leave the burden of proof on them!
If that's too graphic, paranoid, farfetched and nobody likes it....well...
Welcome to the internet SWIM!


localbuilder

  • Guest
KOH Raised?
« Reply #50 on: October 07, 2004, 12:59:00 AM »
Uncle, If not enough koh is being used in many cases.  Is there worse affects by useing to much koh if that's possible?  Second, could a reflux over 30 min. assure a better finish?

UncleFester

  • Guest
KOH amount
« Reply #51 on: October 07, 2004, 03:12:00 AM »
In the example recipe given in my old org chem textbook..Intro to Org Chem by Streitwieser..they used almost twice as much KOH in their hydrolysis as in my original expt. with the Walgreens pills. Since those pills are long ago part of the sewer system, I feel no fear of heading up the river over them. Fooling with sudafed pills to determine their makeup is no crime. There may well be a "too much" point for KOH, but this level isn't there yet.

tina_craig

  • Guest
Swim is a little unsure of exactly where the...
« Reply #52 on: October 07, 2004, 03:13:00 AM »
Swim is a little unsure of exactly where the pill ID is located.  There are 2 bar codes with differing #'s, one on the outside of the box and one if you open the end on the inner flap.  When these were boiled they did go from pinkish red to orange to milky white.  Swim inadvertently overlooked a step in swiuf method, the step of letting the freshly boiled IPA settle until clear.  Swim had 4 more boxes left and decided to start this time with a 24 hour xylene soak.  swim will continue with the rest tomorrow.  Something odd, swim took the last extract and washed with tone, then dissolved in methanol and chilled in frig and then moved to freezer, noticed some gritty stuff in bottom of beaker so let it return to room temp to filter.  What swim thinks is the pseudo just became a milky cloud suspended in the methanol after cooling and after it returned to room temp the cloud remained, also it would float from bottom to top at different temps.  Shouldn't the pseudo have redissolved?  Solid xtals never seemed to have formed.  Is this gear or uncleaved polymer?  Methanol is clear other than white cloud which stays together to some extent and when shaken reforms after 30-60 minutes.


UncleFester

  • Guest
pill ID
« Reply #53 on: October 07, 2004, 12:57:00 PM »
Just the brand will fine for identification. A presoak in solvent shouldn't be needed if enough KOH is in the brew, and do let the flakes settle out. It's a simple and effective way of removing a load of crap from the mixture.

tina_craig

  • Guest
Another thing, swim was reading through all...
« Reply #54 on: October 07, 2004, 03:55:00 PM »
Another thing, swim was reading through all the pill xtrction techs on Rhodium's site and read a few places that letting the PM sit in the ISO IPA too long will allow it to start absorbing polymers.  Does this apply here or does it matter or is swim misunderstanding what was written.  It was in the STE and STB techs.  Only did xylene soak for 2 hours drained and dried and is sitting in 200mL 91% ISO IPA now, figured it sitting overnight in ISO certainly couldn't hurt anything.  KOH is pure from chem supply and will boil these last 4 boxes down this evening.  So 96 pills + 10 grams KOH?  Would it hurt to use 12 grams?  Another question, on future xtractions, swim is going to pursue some white 60's because swim had very good luck with these using ISO and evaporated drain cleaner, could swim use methanol instead of ISOIPA?  The KOH as understood is soluble in alcohol.  And one last question, would it be easier and more efficient to only do extractions in 100 pill segments or is it worthwhile to do 400 or 500 at one time?


UncleFester

  • Guest
Ican tell who..
« Reply #55 on: October 08, 2004, 02:17:00 AM »
hasn't bothered to read through the thread before doing experimental. Did it save you time? No, it wasted pills, effort, danger and money. The Chemical God is pleased that it also didn't cause polluting solvents to be spewed in a wasted effort. Read the thread and follow directions. Then your problems will be solved. If you would like a shorter summary of the thread, SOMM 7 is out in a few months. If you would like to invent your own method, feel free, but I think the experimental on this one was done well. I only get cranky when it is obvious that the experimenter hasn't read the text.

tina_craig

  • Guest
Thread was read...
« Reply #56 on: October 08, 2004, 02:52:00 PM »
Swim read entire thread it is just so long it is hard to retain it all, it took swim 4 hours to read entire thread if that tells anything.  Sorry if the questions seemed whatever.  swim remembers reading something about methanol in thread and will just search it out.  Nevermind.

Was going of a publishing emergency, but read ALL OTHER experiments. Sorry to bother.


Jacked

  • Guest
reply
« Reply #57 on: October 08, 2004, 03:46:00 PM »
Relax, one day you will understand his frustrations and if not it is a small thing compared.. Methanol? The key to this whole KOH method is "hydro" Water in short. 91% IPA contains 9% water which has a key roll in this method. A substitute will create more problems that will only generate more questions and lead the technique into a totally different extraction method, in turn this will even confuse things more turning a gift thread into a hard to follow mess of try this or try that with no confirmation on anything. Miss one post and you got to start over. Your 4 hours turns into 6... Sometimes a break from everything is in order to reflect on what you have read and after a few days relaxing it will hit you like a ton of bricks... Trust me on that.. Relax.


tina_craig

  • Guest
Thanks Jacked, wasn't trying to be shitty with
« Reply #58 on: October 08, 2004, 06:17:00 PM »
Thanks Jacked, wasn't trying to be shitty with anyone, just got frustrated which swim is sure is a regular occurence round here.  Will stick to do it by the book technique.  Sorry uf.


UncleFester

  • Guest
reading list
« Reply #59 on: October 09, 2004, 04:16:00 PM »
There are three experimentals which are required reading. The original exp headed Publishing Emergency using Walgreens generics, the later one using brand name red hots,and the following one using Walmart generics. Walgreens generics are formulated exactly according to the Patent, and hydrolyse nicely using maybe 7 gr KOH per 100. The brand name pills are a more advanced formulation which plugs filters, and produces a milky suspension when hydrolysed. This formulation benefits from using around 10 gr KOH per 100. Then with the Walmart generics, it was found that they are virtually identical to the brand name formulation. One can assume that many off brand generics will also be formulated in a similar manner. It was also found in later experiments that solvent presoak isn't required except in the case of 25 mg ephedrine and 200 mg guifenesin pills. A soak in toluene to remove guifenesin is required with them. One could expect similar results with sudo pills containing tylenol.