Author Topic: Problem gassing generic 120's  (Read 46507 times)

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Scottydog

  • Guest
Polysorbate 80
« Reply #80 on: May 11, 2004, 06:47:00 AM »
Polysorbate 80 has to bee the culprit.

Swim tried using more NP and less pills per carafe as recommended by Geez and still ends up with pseudo that registers with a ph of 10 after filtering off the crude pseudo and mixing with water!

As mentioned in another thread concerning Polysorbate 80, these end effects match the symptoms.

The added titration step cannot bee avoided with the 120's!

If one simply gasses the NP after employing the tetra trap, filters, dry and then runs this crude product, he may very well end with what Geez describes above.

By employing this added titration step with FRESH NP and dh20, after adding muriatic until the water layer reaches a ph of 6 or lower. Some of this residual gakk will stay in the NP layer, while some of this remaining crapola will form at the interface.

This water layer is then filtered again through Charmin TP and THEN evaporated.

If one just chooses to gas, dry and then shortcut straight to the reaction, of course this residual gakk will find its way into the end product.  ::)  

There is something to this added, once thought to bee unnecessary, titration step!

Like any of the other write-ups on this board, any shortcuts usually spells disaster.

As Swim has mentioned before, he combines pills of SIMILAR inactives. 2 different store brand 60's containing PEG, mixed with the 120's doesn't pose any problems with extraction.

If all else fails, after doing a tetra trap, evaporate the NP down to a skin, allow to completely cool, decant the yellow liquid gakk layer from the freebase, then titrate this FB to get the salt.

Tetra, 120's and sodium carbonate are still selling out in the aisles, so it must bee working for others. If Swim doesn't wake UP early enough, he has problems with acquisition.

Sorry you had less then superior results.  :P


ChemoSabe

  • Guest
Further Weirdities from the new 120's
« Reply #81 on: May 14, 2004, 09:47:00 AM »
Swim's buddy had been on a one batch per month schedule this year and had what he had thought were the finished and petered out lye water and naphtha for his March and April batches just sitting in separate flasks in a cabinet waiting for eventual recycling.  Just for the hell of it one day he unstoppered the April flask and lo and behold it reeked of that characteristic fishy freebase fragrance.

This April batch had been older era pseudo that was been mined from past but not quite complete extraction endeavors but the batch itself had been tainted by residual gakks (most likely hiding out in the used but still cleaned RP from the March batch.

A titration was done and about 3/4 of a gram was pulled from the old naphta layer. The quality was OK but it was bordering on what I call "jawclentch junction".

Next the older March batch was uncapped and it seemed to reek even more than the APril. So the naptha was separated, rewashed and titrated and this one was a big surprise.

The March batch had been swims buddy's first run in with the new hyper gakks and it is what he is refering to prteviously in various posts within this thread.

He expected its results to be worse than the April batch but he was pleasantly surprised. It was top grade shit!!! Far from any junction of jawclench and rocked up (or is that cracked back?) good and proper in a borosilicate vessel of vaporization.

I think PappyEarthApple had a related but not identical incident occur that he mentions somewhere in this thread.

But it appears that the lye layer holds on to a portion of the yeild that it later releases. And at some point that chunk'O yeild becomes a completely freed former hostage from the super gakks.

So maybe if you let your based rxn just sit around for two months you'll end up with spanking clean product.


UncleFester

  • Guest
head banging
« Reply #82 on: May 15, 2004, 02:07:00 AM »
My God...just this sort of solvent playing is what the inventors of these new generation of pills had planned...it will frustrate you forever. The polymers must be attacked and disarmed, and other approaches are a waste of time. Boiling KOH in alcohol (not anhydrous) does wonders...why back to this solvent approach?? This has worked for me, and others,..why continue this avenue. In reply give specific experimental details.

Scottydog

  • Guest
Decanting coffee colored fluid
« Reply #83 on: May 21, 2004, 02:19:00 AM »
Swim changed things UP a bit this time and opted to try odorless mineral spirits with a fresh batch of generic 120's.

No pre-cleaning as usual and employed the tetra trap extraction method.

Swim noticed the coffee filters werent as full as usual after having simmered in the NP for 20 minutes per pull.

The extractions pulled alot of yellow precipitates after drying and gassing. After wringing out the sludge and titrating had to decant off a coffee colored gakk fluid.  :o

Swim doubts it has anything to do with the decision to try a different NP but more towards what Geez was saying.

Looks like Swim got the last of the good 120's during the last extraction and the crapola has arrived.

The adulterants obviously hit Geez area first.

Swim is contemplating revisiting the 120's at another time and doing Wareami's "news flash blue streaker UP" prior to the tetra trap to see if this kills the crap.

Ya never know, Swim saw the worst of shit hit the blue 60's before all others. 120's have always been more available, guess it doesn't really matter anymore.  ::)

My apologies to Geez and all other bees for a method that without pre-cleaning may have now become obsolete.

Those pill fuckers work quick eh?

Japtetratone/purplepoison... ;)


Shane_Warne

  • Guest
misc. simple advice.
« Reply #84 on: May 21, 2004, 10:20:00 AM »
Try spending 3-4 hours on mixing vigorously and gradually elevating the heat.
Use a 80:20 mix of naptha and mineral turpentine. He does this to ensure better pfed solvency at all phases of the warming process.

The 3-4 hours is where we differ I think, and I have a feeling you people use larger batch sizes.

tetra isn't used either, clearly such a powerful solvent, miscible with your NP (it is) is going to pull a host of stuff. Just like using alcohol as your basing medium does.

Same with DCM. There is just no way you are going to get a clear extract using something like that, it just makes life harder.

SWIM also uses a sprayer to introduce water over the 3-4hr period. With a mist you ensure that the top layer exposed to the non-polar is based first.

using a skewer to rapidly create narrow lines in the sand also helps with that.

SQuashes the pillmass on the final pull with a coffee plunger.

filters out all the "floating clouds".

separates the tiny basic water layer.
washes with a tiny amount of fresh water once.

horses for courses though, I've been known to get it wrong, but the yields are certainly clean and nothing to be upset about. 60 and well up.

a rinse with wet tone/h2o mix and some fancy evaporation plate shuffling work should make you hit the final opponents for 6 runs.
(But don't look at the crystals too long the glistening pearlescents can damage your eyes when it's too clean!  ;D )

geezmeister

  • Guest
almost explains
« Reply #85 on: May 21, 2004, 04:29:00 PM »
Wow, Shane. You almost describe what you do. And almost tell us the pills you use. And almost tell us what you base with, what you extract into, etc.

All of which seriously limits the usefulness of the information you impart.

I'm not criticizing your method... I don't know what it is. But if you want to chime in and help us with the problems we face... at least be clear enough about what you are doing for us to understand what you are doing. Otherwise, you are just posting advice without practical application.


Scottydog

  • Guest
EudraSHIT and the modified Li birch
« Reply #86 on: May 22, 2004, 01:49:00 AM »
The birchers in Swim's area are still cranking out gear.

So I guess eudragit doesn't interfere with a birch rxn?

To stay on topic, then I suppose 120's are still fair game for the birch and it just may bee the way to go?

I suppose more bees will end up switching rxn methods?


Shane_Warne

  • Guest
clearer I hope
« Reply #87 on: May 22, 2004, 09:30:00 AM »
geez, sorry
Na2CO3, sodium carbonate. (As if I'd be talking about NaOH if I'm describing dry basing) The amount of base is the amount specified in the tetra trap method, about one to two table spoons per gram.

'what you extract into, etc'

I clearly state that extraction is done using an 80:20 combination of naptha (or colemans is fine) and mineral turpentine (not pure, not yellow, but residueless mineral turpentine).

The pills are varied, blue and white 60s are the best, because they are ground easily.

De-shelled 120s may work nicely with that method, but I have my doubts, it's like trying to grind stickly lollies, where the small pieces like to clump together.
But it hasn't been attempted because he operates like this: one box for a method, if successful he buys maybe 3-5 boxes of the same brand to aquire enough for a nanoscale.

Oh but, any crystalline gak that appears as pfed.fb does... I'm uneducated on. But nothing like this has effected anything important.

spraying, mixing as vigorously and as often as you have the patience for, time, and extraction solvent is the secret...which is no secret at all, it's common sense.

I thought I was clear, (1) do a tetra trap, (2) skip the tetra, (3) use a sprayer and not a spoon, (4) aswell take 3hrs to build up to temperature with (5) vigorous mixing with a wet skewer.

(6) Decant the first pull in to an appropriately sized glass bottle, fitted with a funnel and using 1 coffee (7) filter to remove the cellulose vessels (floating clouds...are ya with me?) 

Now spend about 10-20min on the 2nd and 3rd pulls, again filtering through the same filter paper, which hopefully contained mimimal solids from the first pulls filtration.

On the 3rd pull, decant the NP sitting on top of the pillmass as you had done on the 1st and 2nd...but this time (8) use a coffee plunger or other similar implement to SQUEEZE out any remaining NP from the pillmass.
note this has been shown to also bring a small amount of basic water across which requires separation.

Now...(9) Look at your combined layers in the bottle, observe whether it is clear or requires further filtration.

I mean by all means try passing 120s through this technique, but the result Ill just speculate will contain residues of various colourations and descriptions which require rinses.

LAstly, if you do a tiny h2O wash of the bottle containing your NP, don't add H2O to your acetone for the plate rinse.

Well I do want to help, as you queried, but I didn't know how much detail you needed to get you on your way...

weaz1dls

  • Guest
Will try gassing…
« Reply #88 on: May 22, 2004, 09:44:00 AM »
SWIW will try gassing at step g in SWIW’s procedure and post the results.  Hopefully they will be a positive note here.