70% plus yield, clean p/fed is still possible

[barkingburro]

ok here's this weekend work that was rather wonderfuly succesful



123 boxes of 24 count white 60's with chlor
60ml of anyhydrous ipa per 2 boxes
10ml of 91% ipa per 2 boxes
hcl 34%
sodium bicarbonate

charmin
filters
pie plates/evap dishes
grinder
beakers
hotplate
ph strips


-grind pills to a fine powder.

-mix 91 and 00 ipa's in a suitable sized beaker. heat to    100F or 40C.

-add pill mass to heated ipa. stir and then remove from heat. allow pill mass to settle then decant.

-heat and add the 2nd 1/3 of the ipa to the pill mass and repeat last step, combining the two decanted ipa pulls.

-repeat with final 1/3rd but allow to settle till clear.

-take first 2/3rds and filter through charmin plug. when filtered decant remaining 1/3 that is now settled to clear, and once filtered then filter entire wet pill mass. set aside mass until sure all p/fed was pulled.

-bring ipa/pfed mix to 100F/40C once again in a beaker, and once at temp add enough hcl to bring ph to between 2 and 3. once ph is reached let simmer at temp for 20 minutes.

-while stirring add several tablespoons of sodium bicarbonate a little at a time. mix will foam and sputter rather well, but keep stiring and it wil calm. ph was brought to 5 and as high as 7, both worked comparably.

-let solute now simmer at 100f/40c for another 30 minutes or until all foam has died down. stir as needed. mixture should now have a yellowish tint

-filter heated mixture and pour into pie plates or evap dishes. and evap as to your desires. rinse with MEK. swibb both evapped and rextaled. the rextal seemed to be a bit cleaner and swibb used MEK in place of acetone.

some of the later pulls from the evap dishes was a lil gaaked, but a quiick 3 - 5 min boil in MEK took care of most of the issues. MEK was tinted yello as well after boils and a yellowish oil was noticable stuck to some of the filters of the later pulls.

in swibbs experiment he used 123 boxes, that is 177.12 total avail. he returned with 128g of clean p/fed that reacted quite nicely.that's 72% yield and swibb thinks it can improve from there. there was some evidence of gaak, but not much, it came through the rxn as a yellow scaly chunky stuff that floated on top. it was pretty easily filtered out. still finishing the work up so no final number on the rxn yield.

[NaXen]

Its nice to see such great returns with such a simple method, good job!! be sure to post the final results and yields!   why the mixture of anhy. and 91% IPA? is the small amount of water kept in order to break down pills?

[psilly1]

Swip just did this on generic redhots. Did acetone on wash after xtals. Looks good so far. Interested to hear how rxn go though. Swip is doing another run. No sign of yellow oil yet!!

[12cheman12]

Do a burn test on the pseudo and tell us how clean it is, swim really doubts that its as clean as you hope.

[psilly1]

It's not as clean as swip would like it, but better than what swip had two days ago ! Progress none the less.

[barkingburro]

swibb pulled 75% from the rxn. with this pfed. its not the cleanest pfed swibbs ever eacted but it sure has worked alot better than most of the other cures hes used lately aside from straight to E. if any flaws are apparant as of yet its that the alkie/pill mass needs to be filtered through a fine filter or charmin plug and that an MEK boil of all pfed rather than just a rinse would be benificial. acetone just wont cut it. the process seems overly simple and therefore must have something wrong with it, but it's working. swibb doubts highly that it'll work well on the 120's but is about to try anyway. if nothing else this is a good first step in an overall cleaning procedure and it sure beats 30% yields. anyway, will get back with more info. for the record swibb is beginning to wonder if the application of a base to a strong acid or visa versa is somehow responsible for dismantling the gaaks. in festers work up it's a strong base applied to a weak acid and the opposite here. could the salting affect be somehow helping the process?

[12cheman12]

bakingburro, the million dollar question is.
Is the feedstock your using infested with the latest nasty gak? the yellow oil that comes through everything.
If it is and your clean got rid of it then its what were looking for, if your pills didnt have this gak then theres no big deal because theres already heaps of cleaning techniques out there to work with those older pills.
Its the new gak fucking everything up now.

[abominator]

In swim's area both the name brand and generics are very nasty, the ones with CM, that only list a few inactives are the ones swim is referring to.

Way to go BB.

[psilly1]

Swip is not sure, but thinks that by dropping to an acidic environment, then raising to a closer to alkiline ph, which from what swip understood from the pdf's on eudragit, it precipitates at ph's from 5,6,and 7. This may look to the gak as if it is going through the digestive track. Ph is not high enough for pfed to free base but maybee the gak may come out. Definitely needs more research. Dont know if swip's pills had/has oil yet but have not seen any. Last batch was nasty and rxn gave poor meth. Did your rxn produce good effect? Swip got some 120's and is waiting to hear how BB's clean goes...

[barkingburro]

swibb's not here trying to tot his own horn, but the process did work on pills that previously had the oil. swibb was also careful to point out that it hasn't yet been tried on other pills, and while yes there ARE slews of other cleaning methods even if there is no oil presentm, this is by far the easiest swibb has done besides a simple  filtration.  ther are no solvent boils, no large amount of heat needed and basically no fumes that would draw suspicious looks. it does take a lil more time than some, but i digress. when the red hots are done swibb will post results. cheers.

[psilly1]

Swip did redhots from our store we all love 24/7. swip is curious about results on 120's. also, about quality of rxn product. Swip's redhots were dated 12/05. dont know if the same. Swip was wondering if after bringing ph up, or a little higher, about 9, then doing a wash with np if that will remove dreded oil, because pfed should not precip until 10+ but oil should?

[Prepuce]

see if you can base it into freebase and get something that will dry. The biggest probelem SWIP has seen is just that. As the hcl salt it looks so clean you'd swear there can't be any gak left. But turn it into freebase and you end up with a yellow puddle that won't dry. If it does dry you can run it through a SPD and it will be just about pristine. If not you don't want to run it through a reaction, because you'll just end up with a mess. At least that's what SWIP says has been happening to him.

It would be great if this works as well as you think it does, and SWIP will be giving it a try.

PP

[barkingburro]

ok, swibb's efforts with the red hots were just as well. 1.1 of 1.44 available. that's 76% tho swibb changed the method slightly, though it follows the same concept. swibb was just about to start a nano, but is taking prepuce's suggestion. will be back with results...
oh and the changes went like this :

heated 140ml 00% IPA (well, 99.45) to 40C
added 48 unground, still red pills
stirred, and while raising temp to 80C added 34%hcl till ph was 2.
stirred and crushed pills with stir stick, and simmered with temp at 80c for 30 minutes once the pills had been broken up.
added baking soda a lil at a time attempting to ph to 7-8 but red from dyes made it impossible to test with ph strips. so swibb guestimated based on previous attempts.
simmered for another 30 minutes at 80c.
removed from heat and filtered through charmin plug still hot. ran 30 ml hot ipa at end of filtration to push anything clingy through.
reduced over very low heat and with a fan until about half way reduced. raised temp and then filtered once more through cofee filter. finished reduction.
boiled solid product for 3 minutes in 50ml MEK, filtered and rinsed with MEK.
after drying was left with a pink/orange pfed.

the orange IS a lil worisome, but the crystals look good. wil base and get back

[Scottydog]

Very good writeup and extraction method!

Simple and OTC. Swim had a dream and in the dream, there was no yellow oil.

No solvent soaks, boils etc. Just baking soda, alcohol and Hcl.

Swim used only 91% isopropyl alcohol!!

5 pints of IPA were used for 50 boxes of white 60's (48 ct) They were a mix of generic 60's containing both tripolidine and chlorpheniramine maleate.

Swim basically used a blender to grind up the 50 boxes. 25 boxes of pill powder in each mason jar. Dumped 1 pint alkie in each jar, shook like hell for a few minutes and let soak overnight.

Swim did not do any actual filtering at first, just syphoned the semi cloudy liquid off the top and dumped into an evap dish. Did this a total of 3 times with each jar until the 5 pints were used up.

Swim took the cap off the HCL bottle and added 1 1/2 capfuls of muriatic to the alkie. Stirred it up and evaporated at low temp until nearly half of the volume was gone.

Swim added baking soda until the ph registered as 5. (4-5 heaping teaspoons) until no more carbonation/bubbling was noticed after additions. Evapped on low for like 5 minutes.

Fresh IPA was added to the soup because some of the cloudiness fell to the bottom as residual pill mass. Swim wasnt sure if some of this was pseudo or not.

Diluted it fairly well with alkie and then fine filtered through charmin. The filtering took forever.

Evapped it all the way down to a skin, then allowed to cool in front of fan.

Boiled/washed 3 times with acetone. The pseudo looks clean, plentiful and O1, O2 and "neo-fat" free.  

Hopefully tomorrow Swim will elaborate a little further as to what transpired in his dream, so we can get an accurate yield report.

Hopefully, Swim will do at least 1 recrystallization with ISO IPA to bee certain of purity.

No KOH or Xylene necessary.

Happy daze are here again!

No more PM's asking for an A-Z extraction method. All replys will get a UTFSE response.  

Its easy to pull a barkingburro and you can too!  

Thanks barkingburro; you rule!!

[12cheman12]

Who ever has done an extraction this way can they burn some pseudo and let us know what happend.
You cannot tell if its gaked by looking at it, Swim has many many times gotten nice crystals but when burnt left orange or black gak behind.
I think after its burnt it should leave the surface looking how it did before anything was even placed on it.

[abominator]

I do believe Scottydog knows clean pfed when he sees it.  I think the main indicator is the yellow oil.  It is the yellow oil that was foiling many rxns and extractions.

Way to go BB and Scottydog.

Now the stores in swim's area will get to move some of their 60s, which had been abandoned as of late for a different feedstock.

Gluecifer is stoked, he is out buying 60s as swim types.

[Scottydog]

Yield was right at 50% after 2 recrystallizations using ISO IPA and acetone. 70gs out of a possible 144.

The crude pseudo, immediately after extracting via barkingburro was "at that time" around 70% or higher by weight.

I imagine the crude pseudo could run through a HI/RP without a hitch because it is the orange and yellow that are rxn foilers and yield stealers. Everything they threw at us before these denaturants, fell off with a post rxn A/B.

Well, at least Swim has dreamt it to bee factual.  

Then again, Swim would much rather do the recrystallizations and save $ on the other precursors. Using the unrefined pseudo, will most likely also give a smaller percentage return in finished product, post rxn.

The foil burn test seems to bee UP to par after the ReX's. Nice and sugary and does not stick to the pan, no funny smell, no discoloration, nor does it take forever to dry.

Swim can now see how the barkingburro, Fester cure, ahgreich (NP evap to get freebase) and the Prepuce (short path distillation) could all entertwine to make for a customized extraction method, producing superior quality precursor.

[Prepuce]

Scotty, congratulations on your success with the new method. Although he hasn't yet hed the chance, SWIP tells me he definitely wants to try it.

He also wanted me to mention that he thinks he's found an easier test for yellow/orange gak, and that is to take a small amount of pfed hcl and mix it with a bit of dry NaOH plus just a little touch of H2O-just enough to dampen it. If it's got gak that should bring out the color.

BTW, SWIP is also with you on the recrystallization. In fact he is becoming a clean pfed freak. The results of a rxn that isn't full of gak just can't be compared to one that is. Then there is the waste of resources you mention, and shitty yeilds. SWIP would rather come out with twenty percent yeild of clean than seventy percent of dirty feedstock.

PP

[geezmeister]

The results of a rxn that isn't full of gak just can't be compared to one that is. Then there is the waste of resources you mention, and shitty yeilds...SWIP would rather come out with twenty percent yeild of clean than seventy percent of dirty feedstock.

Another convert. You know now why I prefer an a/b extraction with a 60% yield of really clean pseudo to a higher yield of almost clean pseudo extracted with alcohol.  There is a simple of rule of thumb involved here: The cleaner the feedstock the better the dope. 

The restrictions on pseudo purchases where I live make it difficult for me to experiment with extraction techniques. I suspect this method could incorporate the step of precipitating the pseudo in hot solvent to great advantage. I have the hunch that the remaining impurities can be cleaned out by precipitating in naptha or a xylene/naptha mixture. Precipitating pseudo in hot solvent removes some crystallization inhibitors. Pseudo cleaned this way usually crystallizes more readily.

[evilscripter69]

this method, SWIE followed through with a test on redhots/eudragit, and also the 120's w/PS80. ended up basifying resultant gakk filled fed to run SPD on it.
Attempt this and most likely you will spend a lot of time needlessly. That is if you are dealing with the new crap in the pills