Author Topic: New Straight to E -- a novel extraction tech.  (Read 68705 times)

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walter

  • Guest
Teflon pans
« Reply #60 on: June 23, 2003, 05:39:00 AM »
SWIM has used a teflon frying pan on the coil stove top as a hot plate and it works great. He used to use an oil bath as well but the pan by itself has proven to be robust for all temps required so far and is a lot cleaner! All solvent fumes are piped away down the drain so sparks aren't really an issue.

johndee

  • Guest
FYI
« Reply #61 on: June 23, 2003, 06:01:00 AM »
SwiJD advises that the mgmt of a certain MAJOR paint chain, and not a little euroboy, is in the habit of "cutting" many store-packed solvents with alcohol...


Glacial_Refluxer

  • Guest
Swim used this same acetone to wash some meth...
« Reply #62 on: June 23, 2003, 07:21:00 AM »
Swim used this same acetone to wash some meth and it did
not disolve any meth one bit.

Maybee the last brand was tainted with toluene or
something.


Scottydog

  • Guest
Some imaginary feedback
« Reply #63 on: June 23, 2003, 08:56:00 AM »
Swim fell into one of his insomnambulistic trips and hasn't (as of yet) dreamed of adding the xylene and after two pulls on 20 boxes of perrigogo 120's has 1/3 of a whistlxr carafe filled with what appears to bee a pristine pseudo "slushee"  ;)

The pseudo does not charge out after the xylene stage at 105°C but rather after the 50/50 IPA/Naptha 2 minute boil and filter (as it cools to room temperature)  Edit: After further dreaming, actually both are true! Pseudo HCL is highly soluable in hot IPA so when the alcohol has completely evaporated, the pseudo mysteriously re-appears in the Xylene. Temperature controlling its soluability if the alcohol is still present.

An extraction with a "built in" recrystalization.  ;D

He imagines that it has some gakk in it and the xylene will cleanse it further? From the looks of the needles settling on the bottom of the carafe, is the xylene step even necessary? Maybe just for pillstock containing povidone?

There is no possible way to get a yield guestimate at this point but it will not bee too far off in the near future.

3 whistlxr carafes.

1 to dry the solvents, 1 to do the pill boils, and the 3rd with a funnel and charmin plug for HOT filtering.

Multiple canning jars to store or temporarily hold the dried solvent mix prior to pill boils etc...

Swim was going to dream of using a canning jar to filter into but feared that it may shatter due to the extreme temps.

A carafe works great for 20 boxes of pills.

Wouldn't recommend going any higher per coffee pot at one given time.

The fluids and pills filled the pot to the 3/4 mark...

So far so good!

The first pull with the 50/50 juice got pretty much every thing there was to get. The 2nd a tiny bit more. He has not pulled a 3rd time and fears it may bee a waste of time. 2 pulls may bee sufficient.

The shit settles EXCELLENT and FAST

The 1st pull had quite a bit of pill sediment in the filter, the 2nd pull practically nothing.

Stainless steel spoon works great to spoon the sediment out and back into the carafe.

Swis continued to use the same funnel and plug but recommends that a bee might bee better off having 3 of them lined up with plugs already pre-wet with the juice and ready to rock. A fresh one for each pull.

Swis used a dual hot-coil from Wally (if using a carafe don't forget the trivet) with a box fan blowing over the top and an open door for ventilation.

The pharmaceutical companies owe Swim in a major way, them greedy bastards!

Some two for one deals wouldn't hurt.  ::)

Hope this helps the newbees.  8)

Gotta love this place/ Gotta respect VE

More to follow...

L&R


Scottydog

  • Guest
After further pondering
« Reply #64 on: June 23, 2003, 10:28:00 AM »
Considering that pseudo HCL is insoluable in Naptha and practically insoluable in cold IPA. (Also there no longer beeing any water present) Swim was thinking that after the 3 pulls with the 50/50 juice and allowing it to come to room temperature, the needles will settle to the bottom and there will bee plenty of extraction fluid on top (not leaving much room for the addition of xylene)

Especially the 1000ml called for in the write-up for 20 boxes.

He figures he will syphon (turkey baste) the alky/naptha/gakk off the top and disgard. At least as much as possible and then proceed with the addition of xylene and the 105°C boil.

Does this sound efficient as a space saver?

Or do any of the elders forsee any significant loss by doing so?

Theoretically speaking...  ;)


SHORTY

  • Guest
Actually isnt it necessary to leave the solution e
« Reply #65 on: June 23, 2003, 04:40:00 PM »
I think the whole point of this technique is to leave everything in the solution cause the alcohol will boil off which leaves nowhere for the pseudo to go so it crashes out.  Then by reaching the temp of 105c, any water that might have gotten in there will be boiled off while at the same time the naptha and xylene are holding any gaaks which go through the filter when hot leaving only the pseudo to be caught.  The gaaks will appear soon after in the dirty xylene/naptha mix while the pseudo sits in the filter all by its self.  At least thats the way i understand it.  If you remove any of the solution before boiling then i would think you would be removing some pseudo as well.


geezmeister

  • Guest
how about some notes
« Reply #66 on: June 23, 2003, 05:23:00 PM »
Geez has been on a more or less self-imposed lab vacation recently and aside from a couple of bumps a week ago has been clean and sober for not quite a month now. This is not to be construed as having anything to do with a moral imperative, but has a great deal to do with with storms, clumsiness, and the errant path of the phos fairy here of late.

what I haven't seen yet is a description of the interface between the polar and non polar layers during the extraction of the freebase meth. That description usually tells a lot about how clean the pseudo reacted really was.
Anyone who has reacted pseudo HCl pulled by this method care to describe the interface they encounter while extracting the freebase meth into non-polar solvent?


VideoEditor

  • Guest
It can bee better
« Reply #67 on: June 23, 2003, 07:45:00 PM »
Hey Scottydog

While what your observing may already be cleaner than what you are used to seeing, you are still only half way there. It can bee better! The 50/50 solution may have started to drop psuedo because of skipping the third pull making your combined pulls supersaturated or you did not combine the pulls at all.  The volume's called for in the method are very specific and there for a reason. The intstructions are painfully anal. By crashing out here and skipping the xylene step you will shortchange yourself on yeild and not defeat some of the more modern super gaks. If the volume of liquid is larger than capacity break it down into two or more passes.

-- THE ONE BOX CHALLENGE --

IMHO getting a high yield from one box is about as difficult as it gets due to mechanical losses and poor lab techique. So here is a test you can do to give yourself a benchmark and proof this method for yourself.

DO ONE BOX EXACTLY AS WRITTEN - NO MODIFICATIONS

Then use this to compare to when you want to experiment so you can see how variations effect the final outcome.

-Peace


VideoEditor

  • Guest
just woke up
« Reply #68 on: June 23, 2003, 08:26:00 PM »
SWIVE just woke up from a recent dream and wanted to share.

3 boxes National Brand 48 x 60mg

potentialy 2.880gr per box or 8.640gr total.
SWIVE's dream yeild was 8.100gr total.
a yield of 93.75%

-- end gloating --

-Peace


geezmeister

  • Guest
Or take the 9.76 gram challenge
« Reply #69 on: June 23, 2003, 08:27:00 PM »
The four box size is very manageable in a single, not-so large container, even after the addition of the xylene. Scottydog's favorite carafe will be more than adequate for the entire volume with room to spare. Geez did the method by the book and from Scottydog's favorite white 60's-- the ones he hits the wall acting about-- and got 9.6 grams of pseudo HCl without being terribly anal about the process. No 98.3% yield should be scoffed at. You do not 'accidentally' extract 98.3% of the pseudo HCl from those pills.

At first I questioned the volume of solvents used, and PM'ed VideoEditor with a bunch of questions which he refused to answer. I had agreed to do the method exactly as written. Having done it once exactly as written, I had no more silly questions and the method made good sense to me.

I still am curious whether our old enemy povidone will come over with the pseudo HCl, and wait to find out whether the orange I or orange II gakks will follow the pseudo. The Orange I should not; if anything it should precipitate in the solvent mix as it cools after the pseudo HCl has been filtered out and rinsed. The orange II is new to me, as I have been on a break from the lab except for the test of this method.


Castortrip

  • Guest
what about the 240's w/ the E all in the ...
« Reply #70 on: June 23, 2003, 08:33:00 PM »
what about the 240's w/ the E all in the plastic pill exoskelaton with just a little hole in the end for the time relase. I just snapped them in 1/2 but that plastic seemed to complicate. Though, It might have been other binders.

geezmeister

  • Guest
your results?
« Reply #71 on: June 23, 2003, 08:54:00 PM »
Castortrip: What results did you have with the 240's?

Glacial Refluxer: If you be shopping for acetone at the big retail store, shop elsewhere. It has been my experience that the brand the boys from Bentonville market will vary in the amount of water it contains, from negligible to downright criminally wet. I will use that brand only when nothing else is available as I have had cans of it I swear were ten percent water. Any time you lose a noticeable amount of pseudo or meth to acetone, the most likely culprit is water in the acetone. I dry all my acetone before I use it as a matter of course. I assume all of it has an unacceptable amount of water in it.


Scottydog

  • Guest
More
« Reply #72 on: June 24, 2003, 12:52:00 AM »
Theoretically dreaming...

After pulling 3x and "allowing to cool completely" Swim went ahead and syphoned a majority of the excess gakk saturated 50/50 juice from the pooled extractions, added the xylene and crashed out at 105C. Filtered the pseudo, washed with MEK and is waiting to get a tally.

Swim will not tally until a dual IPA/tone recrystalization is completed.

Swim figured since polysorbate 80 was present, skipping the Xylene step may not bee the wisest decision.

With the pills Geez is referring to, the Xylene step may not bee necessary because the supergakks have yet to infest that particular brand.   ;)

As for PEG, a recrystalization afterwards with fresh ISO IPA should take care of that problem as most of us here learned way back when tyvek experiments were popular.

Shorty.. Swim agrees with everything you had to say with the exception of losing pseudo.

Swim uses IPA exclusively for recrystalization (red bottle) not dried and rarely suffers any "significant" losses.

Considering that the excess IPA and Naptha are already saturated with gakk, he feels that ditching it won't hurt yields because when the mix is cold, the pseudo is no longer soluable.

The problem with doing this is gakk, making a recrystalization mandatory.

Another observation is during the filtering step of the 50/50 juice. If using charmin, the solvents tend to cool before the liquid can pass. What swim thought to bee pill sediment was actually pseudo.  :o

While waiting for pseudo to dry, Swim started a 2nd 10 box extraction with the 120's and finds that a piece torn from a "blue shop towel" tends to bee a little easier for this extraction technique (allowing more fluid to pass and quicker)

He was spooning it back into the flask and wasting time. Swim now finds it easier to just add it to the pseudo that is filtered off in the end stage and remove whatever gakk that contaminates it through further recrystalization.  :)

Swim forsees that shortcuts are possible depending on pill formulations.

Great thread, great info.

Swim appreciates all the help and constructive criticism...


VideoEditor

  • Guest
laughing out loud
« Reply #73 on: June 24, 2003, 04:44:00 AM »
Scotty you are just determined to do it your own way. . .

Gotta luv ya man

-Peace


Scottydog

  • Guest
Yield report
« Reply #74 on: June 24, 2003, 09:34:00 AM »
Yield Report...

Results are back from Swim's imaginary and theoretical dream!

From the 20 boxes of "12 hour" perrigogo 120mg 20 ct. (48gs possible)

Swim yielded 35.7 gs

Roughly 77%

Pretty good considering that he NEVER uses these pills and could only get them to work once with substandard 50-60% yields using the tyvek method.

Swim is loyal to the foil and the pseudo burns cleanly with zero residue.

Now to see how it runs in an MBRP/I2 dream.

Swim can now go back to his favorite 60 mg pills, less inactives in the carafe, easier to work with and as Geez has attested (Higher Yields)

Sure is nice to know that he can now use the tombstones if he has to.

Kudos to VE and all the bees, test monkeys and guinea pigs who helped to fine tune the technique before unleashing to the masses.


platcat

  • Guest
povidone?
« Reply #75 on: June 24, 2003, 05:25:00 PM »
Swip did  5 X 48 boxes exactly per write up.post rxn fluid ended up piss yellow??interface was very lumpy and about 1 ml thick.
  upon evap mostly pfed was recovered.some minor patchs of diamonds.
   swip is gonna rerun the pfed and see what comes of it.He is suspecting povidone came thru.NP washes of the post rxn fluid all came back piss yellow except the VMP wash which was clear.4 washes of xylene and they were still coming off yellow.rxn had seemingly went well.anybody have any other thoughts??PC


Castortrip

  • Guest
call the feds!
« Reply #76 on: June 24, 2003, 05:51:00 PM »
greg graffin is doin bad things! :o  j/k but that's not too smart unless of course it's not your real name, it's not? oh ok then it's all good then  8)

Castortrip

  • Guest
here's my thought, A/B your STE pseudo next...
« Reply #77 on: June 24, 2003, 06:27:00 PM »
here's my thought, A/B your STE pseudo next time before reacting it.

wareami

  • Guest
Tetra Rinse???
« Reply #78 on: June 24, 2003, 06:53:00 PM »
Platcat: We bees now know that tetra removes POV and friends. It doesn't remove Poo-Tang which is another "Fuckabee in The End" denaturant.
VE: Has SWIVE tried a tetra rinse after the STE?
It couldn't hurt and the time required would only bee the tetra drying time before running the feedstock.
If any invisible poly-inactives are present tetra might be the kicker.
Peace of the REaction
Have FUN-Bee SAFE



VideoEditor

  • Guest
Swip did 5 X 48 boxes exactly per write ...
« Reply #79 on: June 25, 2003, 03:40:00 AM »
Swip did  5 X 48 boxes exactly per write up.post rxn fluid ended up piss yellow??interface was very lumpy and about 1 ml thick. upon evap mostly pfed was recovered.some minor patchs of diamonds. swip is gonna rerun the pfed and see what comes of it.He is suspecting povidone came thru.NP washes of the post rxn fluid all came back piss yellow except the VMP wash which was clear.4 washes of xylene and they were still coming off yellow.rxn had seemingly went well.anybody have any other thoughts??PC

Sounds more like an incomplete reaction. Did you burn test the psuedo before reacting. I have not seen POV or PEG totally botch an entire reaction just reduce yeilds.  So far SWIVE has not seen POV or PEG or Snot come through a STE. Would like to hear how the second pass turns out.

Yes Wereami a tetra rinse is fine if you think somethings getting through. SWIVE does an A/B to freebase and the result is pristine.