geezmeister (Of Counsel)
08-11-04 07:52
No 524846
      last pull yield increaser     

Getting the last bit of the meth from the reaction fluid during extraction is a goal all tweakers share. I was reading the lye lock thread, and thinking that "lye lock" is an outgrowth of an effort to get every last bit of meth out of the reaction fluid. I don't "lye lock," but I do one thing before the last pull from the reaction fluid that does seem to coax a little more meth from the mixture, and its something that doesn't seem to be discussed very often. It still works-- and it may help more now than it used to because of the newer gakks in the pseudo tabs. It may help more now than it did when I first started doing it.

Before you do the third pull with solvent on the reaction fluid, add a capful of 3% H2O2 to the based reaction fluid. If you reacted fifteen or so grams, add a couple of capfuls. It doesn't really take much peroxide to do the job, but the peroxide does seem to work better in a warm mixture than in a tepid one. Stir the reaction fluid well after the peroxide is added, and then let it sit for fifteen minutes or so.

Then add a little more NaOH solution. Ahh! That same reaction fluid that showed no change to the previous addition of NaOH solution now goes milky again when some is added... and the solvent will have a little meth in it when you titrate it.  

If you don't think this works, do your third pull, then add the peroxide, wait fifteen minutes or so, add a little more base, add fresh solvent, swirl, let it sit a while, then titrate to see what you have. Surprised? It isn't going to be a great amount of meth (unless it was a big reaction) but there will be some more meth from reaction fluid that wasn't yielding any more meth.

It could be that the peroxide oxidizes some gakk that is still coating meth HI in the fluid, making it lose its hold. The meth HI is then freebased and available for extraction. If you did a good job of cleaning your pseudo, have a mirror interface, and the reaction fluid bases easily, don't expect a gain in yield. If your pseudo wasn't really gakk free, you have trash at the interface, or the reaction fluid did not base quickly and effortlessly, try a little peroxide. It may help your yield a little.

mostly harmless
 
 
 
 
    abominator
(Hive Bee)
08-11-04 08:51
No 524855
      Great Technique     

Swim has used peroxide in the past in an attempt to break up emulsions, but never too increase yeild like Geez suggests.  Coming from Geezmeister, this is surely a winner and will be employed when swim dreams again.

Wareami once mentioned spraying a shot of TCE to break down emulsions and send the nasties to the bottom, could it bee used in the same capacity as h2o2?

69
 
 
 
 
    geezmeister
(Of Counsel)
08-11-04 09:34
No 524858
      Tetra is a solvent     

TCE is a solvent. Once your reaction fluid is based, it will pull the freebased meth. You can extract with TCE, and if you gas, it is a choice solvent for the purpose. Do wash it very well before gassing.

AGain, the peroxide won't give you a huge gain in yield (unless maybe you didn't have clean pseudo to start with) -- but when you are out, a bump is a bump... and a half a gram is a half a gram more than none at all.

mostly harmless
 
 
 
 
    fierceness
08-11-04 11:17
      Wouldnt it be better to add a reducing agent?
(Rated as: misinforming)
    
 
 
 
    Rhodium
(Chief Bee)
08-11-04 11:51
No 524872
      RedOx chemistry is more complex than pH     

Methamphetamine cannot be oxidized to (pseudo)ephedrine by hydrogen peroxide. Oxidation & reduction is significantly more intricate than for example the concept of acidification & basification

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    geezmeister
(Of Counsel)
08-11-04 13:04
No 524880
      that isn't what I suggest at all     

Adding a little peroxide doesn't affect the meth at all, nor does it reduce pseudo to meth. That isn't what I suggested is happening at all.

Some of the newer gakks buffer pseudo and meth and impede both freebasing and salting out. They are not totally effective, but they are effective enough to have an impact on yield. I noted early on the new gakks impeded a/b extractions of pseudo, and that basing the post reaction fluid took more base, and was less effective, than it had been previously.

If those gakks are present in the reaction, adding a little peroxide to the based reaction fluid, letting it stand a while, and adding a little more base results in a small additional yield of meth from fluid that appeared spent. It will yield a small amount of meth when another extraction of the fluid done without adding the peroxide first did not. Granted, the amount is small. I've done this after a third pull that sat overnight yielded nothing more, and obtained another quarter gram or so of meth. I've done it right after doing three standard pulls of the reaction fluid and gotten a little more meth.

I also have done it with no effect at all after reactions done with pseudo extracted by Fester's KOH method, and after reactions done by two other methods that seem effective. IN each of these reactions, the fluid based readily and quickly with very little base, which was not the case with reactions that were contaminated with some of the newer gakks. Hence my conclusion that the effect is related to the gakk, and the effect of the peroxide on what gakk remains in the mix post-reaction.

I'm not suggesting the peroxide makes more meth. I suggest that it helps oxidize gakks that may be buffering some of the meth present post-reaction from the base and thus preventing its extraction by an a/b process. My explanation of why it works may be wrong, but I have obtained that extra bit of meth too many times to dismiss the effect.

I'm not oxidizing pseudo to meth with peroxide. If the peroxide oxidizes something, it oxidizes a gakk that is buffering some of the remaining meth in the mix, preventing it from being freebased.

mostly harmless
 
 
 
 
    Shane_Warne
(Hive Bee)
08-11-04 14:36
No 524889
      Welldone Geez, Ill file this one too.     

Welldone Geez, Ill file this one too.

Well if there's meth trapped by the end of the 3rd pull, you may aswell try something. This would make that (very) short list at that point, for me atleast.
 
 
 
 
    BullwinkleMoose
(Stranger)
08-11-04 16:45
No 524905
      Getting that last bit     

Geeze is right on abou the TCE: it'll steal some of the FB amine to the bottom

moose has used H2O2 successfully before

But this is his regular course of action,, recently:

thin out the polar with a little H2O,

add a little Goofy stuff removing type of product to the NP ( it has a surfactant in it that greatly inhances the NP's ability to dissolve EVERYTHING (good and bad) )

then carefully microwave until the heating causes bubbling that destroys most any of the interface emultion

allow to settle; but ,seperate while hot
 
 
 
 
    18294
(Hive Bee)
08-11-04 17:09
No 524913
      H202     

I think some of the bees here have been misinformed as to what peroxide can do. Perhaps this is a result of those bullshit cat recipes using 3% H202.

GEEZ- do you think this would help in a post-birch as well?
 
 
 
 
    ozmosis
(Stranger)
08-11-04 18:18
No 524934
      think this would help in a post-birch as well?     

No need really.
Swio semi-dissolves her freebase in toluene then add's flask to ice-bath(stopper attatched of course), ices tank down, adds NH3, starts stirrer and procedes to add Na 1 small piece at a time every 20-30 seconds until all has dissolved then she adds more tolly and pulls flask from ice bath. checking the bottom of flask to ensure all Na has dissolved, she adds dh20(drop by drop at the start(violent reaction)until layers seperate.
She then removes tolly layer, addsmore tolly and stirrs(magnetic) for ten minutes removes tolly layer, combines extracts, dries, filters then gasses(rock salt/sulfuric).
Of 94g freebase she get's ~ 90g lovely smokable honey!
 
 
 
 
    aztec
(exotic beauty)
08-11-04 18:22
No 524936
      geezmeister, you magician!     

only a veteran of this area would appreciate your gift. she understands EXACTLY what you mean and she cannot wait to try this. she knew nothing of this trick. this is timely because for some reason, she has had a much tougher time coaxing the honey out.

in addition, not only has she had problems coaxing it out post-base stage but also at the post-acid stage. what she desperately needs now, my great geezmeister, is a trick to coax it from the post-acidified solution.

not only does she know there is more there because of the yield, but also because there is a distinct smell in which one knows there is more meth to be had. is it an amine smell? she knows that you know to what she is referring. that heavy distict smell after washing the base from the non-polar and adding the acid. but lately, she can't coax it out. she has under-acidified, acidified to perfection, over-acidified. she has heated the xylene, the water, and both- all to no avail. is there a secret here that you can divulge?

she sure hopes so, because given her transient nature at the moment, it pains her to find another safehouse in these times of uncertainty.

regards

Free Speech Free Choice
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
08-12-04 00:22
No 525007
      reply     

Nice job geez. Peroxide is used in the kerplunking technique, the post reaction fluid is hot and based to a pH of 14, Adding H2O2 was always thought to kill broken or unreacted pseudo leaving you with a better product. Yields have always been high doing it. At the time no one realy knew exactly what the H2O2 was doing but you could see it doing something thats for sure. Your explanation could be the answer to this old question some of us old timers have..Doing a third pull sometimes would yield something but in most cases Swim would ended up with salt.  The lye lock always happens when the flask cools though. I cant recall ever pulling off the lie lock after it was cooled off, who knows how much was tossed..

Tighten Up!  (UH)
 
 
 
 
    CharlieBigpotato
(Bizarre pHomme de Terra)
08-12-04 08:21
No 525065
      space and time?     

exotica;
it might bee helpfull to consider distance in the equation:
some travling time is needed. viscosity comes into play in this; molecules move slowly through thick and gooey solutions; especially in a tall beaker or funnel. heat can move things faster and thin out gooey-ness.
or, one could have an excess of dh2o..ensuring a thinner soup for molecular transportation.
the 2 layers can bee transferred into a shallow pan, wherein the distance beetween them is minimalized. then, after a brief wait; dumped back into a sep funnel; etc.

i hope this makes sense.
 
 
 
 
    geezmeister
(Of Counsel)
08-12-04 10:06
No 525073
      patience pays     

Aztec: Save the solvent you titrated. Hit it again the next day. Add some water, check the pH, add a drop or two of acid if it needs it, shake it up, give it time to settle out, and evap it. Some times you get a little more product. I've added water for a final pull and let it sit in the sep funnel, checked it hours later and found the pH higher than the previous pull. I've had an extra water pull produce a little additional meth-- sometimes with a drop or two of acid, sometimes without. This may be caused by the same a/b inhibitor breaking down. (It may be proof that I've been rushing through titrations.) smile However, reactions of pseudo extracted by Fester's hydrolysis method, and with pseudo cleaned by successful Short Path Distillation, have not yielded additional meth from a delayed final pull. The gakk that impedes freebasing the meth may also impede salting it out as well. You might even want to try add a few drops of peroxide to the water on your last pull. I haven't tried it, but it may have an effect on the inhibitor at that stage of the process as well. 

Jacked: Ker Plunking uses peroxide at the outset, while basing the reaction fluid. I still added peroxide whenever I had a less-than-mirrorlike interface in a ker plunk.The idea to add a little peroxide comes straight from the Ker Plunking thread, of course. What surprised me was that after three extractions of fully based reaction fluid,  adding a little peroxide then later adding a little more base resulted in the reaction fluid turning milky again. When I have seen that happen, I have gotten more meth.
I haven't seen this happen with clean pseudo, where I see a mirror interface and the fluid bases easily with very little base-- (like you like it.) This suggests to me the newer gakks are involved, and the peroxide helps loosen their grip. 

Nothing I've seen indicates there is a reason to delay adding the peroxide until after the extraction. In the recent extractions, it has been an afterthought. The addition of peroxide as the reaction fluid is being based (as in the ker plunk) should have the same effect on yield. If you add it as you start the basing, you won't see the additional flush of milkiness at the end, but you problably won't need to do a fourth pull for a little extra yield, either.  As I noted at the start of this thread, this isn't a new idea, just one that hasn't hasn't been discussed recently. Probably makes more sense to add a capful of peroxide early on, although experience indicates its also of use later on. 

Like you, the lye lock I have experienced occurred with cooling after a ker plunk. I've only had it happen a few times doing a ker plunk, to be honest. I have had a little more yeild with a final extraction with xylene after allowing to sit on the reaction fluid for a day or so-- but only where I had less than really clean pseudo to react.

mostly harmless
 
 
 
 
    LoW_JacK
(Hive Martyr)
08-12-04 12:11
No 525085
      Re: Won't H2O2 just oxidize whatever substrate     


Won't H2O2 just oxidize whatever substrate it affects back to pseudo, resulting in a pull of pseudo?




Ahhh yess! I've heard similar bullshit out the mouths of inexperienced cooks vommitting such drivel as they ph their batch in effort to give themselves a window to crawl through if in fact their blunder of a batch turns out to be unreduced pfed instead of meth.
It's quite ammusing to hear a grown man stand by such proclamations and defend their misinformed viewpoint to the extent of violence (if need be).

That post was rated 100% correctly. You've been misinformed and your post is misinforming. Good call.


http://www.dodgeit.com
 
 
 
 
    dwarfer
(esoteric)
08-12-04 14:27
No 525101
      patience, peroxide and paydirt     


Very interesting.  I've seen Marvin's steaming manouvre
obviate the issue, but also recall my own results before
giving up on the Devil's Drug, and I think this technique
would have saved some prostate probs arising from over-exposure to pseudoephedrine.
(Cough)

I had an aversion to it's employ probably associated with
the sideways sneer i cast at Worlock's implication that
the "Ker-Plunking" technique allowed the broken
molecules to re-assemble in accord with their "true and
inherent" manifest destiny to become Meth-Amphetamine Molecules:
thus showing how utilitarian techniques can be
flung aside by attitude alone.

==========

Patience?  Ah yes:  not my natural bent:
but there have been times that I've looked into bottles
of well-gassed and filtered NP:

months later, after it evapped to dryness:

and found shards of apparent beauty laying there,
along with dead flies, and spider web remnants..

A quick wash with a swirl of 99% Iso, thru a filter
into a Test Tube:

quickly blown dry by exhaling thru the Sucka Tube
assemblage:

then inhaling as the fumes commence::
yowsa:
iso-flavored MA fumes:

Big Whoop!laugh


dwarfer
 
 
 
 
    wareami
(Hive Addict)
08-12-04 15:23
No 525109
      Green Tides and High Grass?     

Never a problem for the fearless "DEEP inuENDdoh!" Bees determined enough to exhaust every possibility until resolve lights the way.
More often than not, Ibeeware's found himself floating around the deep end in search of solutions and for the most part, the solutions  usually found in threads such as this, are critical to continued success.
Good Call Geez for giving this subject the airplay it deservescool
While cruising along full sail, content with our growing arsenal of aquired Ware-With-AWE gaakblaster demolition tools, The ImperialGAAKNavy launch another fleet of inactive-dingy's in the hopes of intercepting the piratebootyhunters bounty therebye rendering Roger UnJolly for yet another Legless HI-Seas Adventure in the DEEPEnd.
With each deployment of the major encapsulating Gaaks since Povidone, Ibee always re-lyed(pun intendedwink) on the suggested "last resort" workaround untilizing H2O2 to oxidize gaakbased-emulsions.
GAAK isn't an "IF" you run into it proposition that may or may not require a last resort workaround.
GAAK is a "WHEN" guaranteed obstacle and demands innovative workarounds.
Without the Foresight and Creative Sparks from the master veteran bees like Jacked, Worlock, Geez...et al, we'd bee  gropin more and graspin lesstongue
(reminds me of ole ChesterCopperPotlaugh)
"Arrrr Fukin! Ware's me legs?"
I've included some relevant links that deal with Ibee's first hand experiences using H2O2 post rxn.
The term Keplunking didn't always apply to how Ibee untilized H2O2 in times of need because sometimes heating and salting out were not employed. A simple H2O2 addition to the based postrxn fluid would break the emulsion.
Post 308354 (wareami: "Base the hell out of it! Sorta!!!", Stimulants)
Post 330997 (wareami: "Halla-lu-lu-YAH!", Stimulants)
Post 434955 (wareami: "Paying Attention=Insert Coin", Stimulants)
Post 435045 (wareami: "Green Grass and HIGH Tides", Stimulants)
Post 441758 (wareami: "I've fallen and I can't...kerplunck! :•þ", Stimulants)
Post 441963 (wareami: "Listen UP!", Stimulants)

The CabFair MethodPost 249365 (wareami: "Re: freebase won't go into tolune layer!", Stimulants)
was employed successfully before Ibee learned of Kerplunking.
TCE is a nonpolar solvent...yes!
It's a bottomlayer NP in aqueous solutions.
It's also a great Polymer trash collector.(Hence, the need to wash the TCE/FB before titration or Gassing when TCE is used as a single FB extractant)
A balance was achieved untilizing a dual solvent extract of the postrxn solution when povidone locked up the goodz.
This method failed with Toluene and Xylene but worked like a charm using naptha as the primary solvent.
A ratio of 1 part TCE was added to the basified polarlayer in the presence of 100 parts Naptha as the top layer and the emulsifying trash absorption effects of the tetra pulled the trash while preventing the amine from migrating into the trash laden tetra.
How's that for diggin deep?
So thee moral of the story here is
"When Navigating around The DEEP inuENDdoh! always cum prepared with a large shovel cause it's a Sink or Swim World ya Sea bee for ya!blushwink"
GOING UP????tongue

Remember, it's not,
"Hi, how are you?" it's
"How high are you?"
 
 
 
 
    geezmeister
(Of Counsel)
08-13-04 02:21
No 525130
      that last batch...     

Another good one, eh?

laugh

mostly harmless
 
 
 
 
    CharlieBigpotato
(Bizarre pHomme de Terra)
08-13-04 02:38
No 525132
      intereting one, wareami     

an np on top and bottom sounds fascinating, though only one could bee mixed w/ aqueous layer at a time.

swim has also had luck w/ the last pull occuring a month or too down the road.
um, this H2O2?
i'm assuming is 3%?
can't help but wonder if the extra water is also helping. the tendancy seems to bee to limit water quantity to minmize evap time, etc. leading to those thicker solutions that aren't as "open" to taking on migrating moleules.
ever try a large excess of hot water for last pull, and let it evap for  week?
 
 
 
 
    wareami
(Hive Addict)
08-13-04 06:25
No 525184
      YeeeeeeeeeeHaaaaaaaaa Geez!     

YeeeeeeeeeeHaaaaaaaaa Geez!smile
How could ya tell???
Ohhhh Wait...I know!
Musta been my multi-talented skill of typing and pissing Osmium off at the same time!blushlaughwink
I'll have to keep that in check following the next GoodazitGhetto's BlockParty<____(that should read "HoeDown" but didn't wanna scare BigIdahoChas Off)shockedtongue
Takin Care`O`Biz...you know how it iswink

an np on top and bottom sounds fascinating, though only one could bee mixed w/ aqueous layer at a time.



This would be the case if the NonPolars were miscible with each other.
In fact...that miscibility scenario is what determined tolly and xyl poor co-solvents alongside tetra for this procedure.
Naptha however stayed on top of the Based aqueous layer while Tetra added to solution made a beeline straight to the bottom carrying the encapsulating gaaks with. This created three distinct layers.
The key was to add only enough tetra(~1-3ml depending on emulsion amount) to allow a full saturation with polygaak into the tetra.
If headroom was left by adding too much tetra, then the amines would become confused by their affinity for any NP and hop in the sack with the first thing to cum along!blush
Whoever said that size doesn't matter hasn't fully explored the erotic potentials exhibited by overly-stimulated confused molecules.cool
Pull UP a Couch sometime!wink
Better yet...I could have my shrink call yer shrink if I had one but I'm too busy shrinking sexually confused promiscueis molecules to schedule an appointment with onelaugh
Not that I need a shrink or anything like that...you understand!
It's not like I'm sexually attracted to confused molecules..I just understand their needs is AWE.............
YEEEEEEEEEEEEEEEEHAAAAAAAAAAAAA!!!
HEY...where ya goin??
Was it sumthin I said?
I put the hoedown already...what else do ya want?
Now look what ya did...ya woke the littleguys UP and they're chili now!
laughsmiletongue




Remember, it's not,
"Hi, how are you?" it's
"How high are you?"
 
 
 
 
    Prepuce
(Hive Bee)
08-13-04 15:34
No 525255
      Another thing that helps     

Another thing that often helps after a "dirty" reaction is to filter the post reaction fluid after basing, before gassing or titrating.

PP
 
 
 
 
    geezmeister
(Of Counsel)
08-13-04 22:26
No 525306
      do you mean     

filtering the based reaction fluid prior to extracting the freebase meth?

mostly harmless
 
 
 
 
    Prepuce
(Hive Bee)
08-23-04 04:43
No 526896
      re: do you mean     

"filtering the based reaction fluid prior to extracting the freebase meth?"

Yes, thank you, that's what I meant. Especially before a second pull. SWIP has found that clearing away the particles that tend to accumulate after basing allows for better/more complete pulls. (Not that this is likely to be news to you.)  SWIP has even been known to filter both the based post reaction fluid plus nonpolar solvent, on it's way into the sep funnel, prior to gassing, if it contains solids. He thinks it helps increase yeilds.

PP