Wrong turn on the road to meth!

[snoozer]

OK so swim finished his 48hr LWR and planned to distill his honey after basing the reaction fluid because he's not too confident with the A/B. First off he boiled the reaction fluid to drive off any iodine. Then it was all down hill from there...
First mistake: swim forgot to wash the filtered honey with NP. Big mistake because the reaction fluid was bright piss yellow suggesting contaminants?
So swim proceeded straight to basing the reaction fluid expecting to see honey floating on top of the water. He checked the pH with papers before basing out of curiosity yep it was 1. He added about 170 mls of lye solution (probably close to saturation). He noticed it turn milky white in splashes then stay white completely. Before long swim made mistake number 2: he shook the flask to mix. Before long, yep you guessed it: HUGE EMULSIONS FORMED!
So swim tryed leaving it alone, hoping it would all go away . When he returned it was still there mocking him, upon closer inspection swim noticed needles of some sort clinging to the inside of the flask!. He checked the pH and it was 14, so swim is wondering could this be lye lock? on a positive note it does smell like unwashed pussy though!
Right now swim has a bowl of oatmeal porridge staring at him, the emulsion is REALLY baad!
Swim needs some advice on where to go from here. Should he add some NP to the sep funnel and hope he extracts some meth (albeit dirty) and continue with an A/B workup?
Swim really hopes all this is a result of missing the NP wash and nothing more sinister.
Swim has worked too hard and long to let this diversion stop him from reaching methville.
Any directions would be greatly appreciated!

[ChemoSabe]

I'm way too tired to be any good help right now and I've been having some "eye challenges" apart from that but did I read correctly that you added 170ml of lye solution? If so that is an utter heaping buttload!!!!

50ml or 60 should usually get you a decent enough approximation of lye lock to be safely into high-pH land to get the freebase well into gear on its way towards non polar migration. usually enough of it has made the journey after 1/2 hour to then take some of the NP off the top to water wash  and to then give an initial titration test to see if anything is really there.

I'd need to be more awake to do a proper job of evaluating what's really happened but just for your own education's sake read up on this method of basification. It should help you to round out your basification education even if you never actually use the technique which is described.

Really good emulsion info there too but that's just a samll portion of the value there.

Post 59240

(Worlock: "Ker Plunking for quality and quantity", Stimulants)

Post 377287

(ChemoSabe: "Das Ist Der Kerplunker", Stimulants)

good luck with your batch there and most likely it's OK and salvagable but I'm too far into dreamland to be of real practical help right now. Crash city here I come.

PS what you really need for this is advice from a seasoned freebase distiller which I'd never claim to be but in the mean time it wuldn't hurt you to check out these posts for your general info.

[snoozer]

OK, so perhaps swim was a little heavy handed with the lye! He noticed the solution turned milky white long before he finished adding the lye solution. So it could just be a case of severe lye lock? What could those needles be then? Thanks for those links chemosabe, very informing. Would swim be wise to try the ker-plunk then? or simply dilute with more water?

[auntyjack]

definitely overbasified...read geezs stuff

[geezmeister]

Adding hot water will unlock lye lock, if that is a problem. Add some hot water and pour everything, non-polar solvent, emulsion, polar layer--- in a big enough pot to heat it all up slowly.

As Chemo suggested, this is a good spot to use the ker plunk method.

There are some notes on fighting emulsions during a kerplunk in

Post 428410

(geezmeister: "The post-reaction workup: a cook's summary", Stimulants)

Everyone does this a time or two. That emulsion will teach you two things: 1) you don't want to shake the nonpolar and based reaction fluid together, and 2) if your are patient, you can recover from a lot of mistakes like this one.

Emulsions will break down with time, and most of them will break down with a little gentle heat. Be patient. If you can stand the wait, just put the stuff in quart jar with a lid on it, and let it sit. Take your time with the emulsion. Most emulsions will separate as the bubbles break down and you should get two layers again.

If you have an emulsion from hell which will not base at all, remember the meth you have in that solution is freebase. Simply evaporate all the solvent and water out of the emulsion, and when it is bone dry, cover it with nonpolar solvent and stir well, let settle, decant the solvent, wash it, then salt out the meth.

[auntyjack]

if he hasn't added a non polar yet wouldn't the solidifying he is refering to, which is happening in the diluted rxn fluid, be called lye lock....which asks the question:is a lye lock an emulsion?

ps.these questions are not rhetorical...

[ChemoSabe]

Those crystals you saw were Lye or sodium hydroxide which was so supersaturated in the water that it started to erupt from it in crystal form.

It's literally Recryst of the NaOH variety.

[geezmeister]

Auntyjack is right. I ASSUMED there was an emulsion formed with nonpolar. Closer reading did say no solvent had been added.

By all means add hot water. This will dissolve the locked-up mess you have. The crystals are likely a mix of NaOH and sodium iodide. Add hot water and let the mess soften then add more with stirring until the solids dissolve. Give it time to dissolve, stir with some patience. coax it back to a liquid state rather than forcing it. Then extract the meth oil with nonpolar solvent three times, combine all three volumes of solvent, wash first with a 10% soluton of NaOH, then with hot water, then cool water. If the cool water wash feels slippery, wash with more warm water.

Salt the meth out of the nonpolar by gassing or titrating.

Sorry for not reading your question a little closer this morning.

add some nonpolar solvent and

[SHORTY]

In the first sentence of the first post in this thread snoozers says he plans to distill.  If this is the case then lyelocks/emulsions are irrelevant.  The needles you see are lye because you added way to much but that will not do any harm.  Thats what makes distilling such an easy, no way to fuck up method.  Although the answer can easily be found in tfse, if distilling, do this.

1. Wash the solution with np.

2. Make a 50% solution of naoh and add 10ml portions swirling (don't shake!)the contents between portions.  When there is no color change (usually white) when a portion is added then stop adding. 

3. Distill the fb.

Any emulsions/lyelock etc. will bee irrelevant once the solution starts to boil/distill.

[ChemoSabe]

Shorty was an ideal person to answer what had been the unanswered distilling portion of this mystery.

That's great info Shorty that a simple distillation can pretty much take care of the whole shebang.

Swim's buddy needs to try freebase distilling some time.

One question.

Does the freebase, once distilled, have that same classic "fish market" odor that one usually associates with a "batch gone good" which is the hoped for scent directly after basification?

I recall Rhodoium once mentioning that the distilled freebase could then be vaporized straight up with out conversion to a hydrochloride salt. I am then curious if this freebase, if consumed in vapor form, also would have that fishmarket flavor while that vapor was being inhaled.

I used to think the fishmarket scent had purely to do with the lye but my suspicions now are tending to think it's true source is the freebase.

Also, anybee know if a Dean Stark Trap would be an advisable peice of glassware to do freebase distilling with? They look cool but I've never been sure if they would be optimal for this use.

Dean stark distillation traps

[Rhodium]

Also, anybee know if a Dean Stark Trap would be an advisable peice of glassware to do freebase distilling with? They look cool but I've never been sure if they would be optimal for this use.

No, if you would use such a piece, there is no way you could measure the vapor temperature and hence know when to stop collecting distillate. Anything with a boiling point higher than that of meth is NOT meth, no matter how much you want it to be, or how alike it looks to the fraction before.

[snoozer]

So if the solids are just lye/sodium iodide crystals, then couldn't swim just dilute with more water until they dissolve?. Then hopefully there would be a milky white solution with oil floating on top like before I went too far with basing right?
So then swim could just distill the water/freebase mix like originally planned.
Shorty: Are you saying to extract into NP and then distill the NP/freebase mix? Maybe I've misunderstood.
As AJ asked, I'm not sure whether I have lyelock or an emulsion or both?. Hopefully only the former.
Thanks guys for your advice, hopefully I'm almost there!

[ChemoSabe]

At the pH which the solution now has NP washings might actually suck up the FreeBase since it would be quite attracted to a non polar environment and would serve to extract it now rather than clean it of residual iodides.

So I think maybe Shorty meant to _now_ proceed with a distillation and _next_time_ follow the post reaction steps he gave.

But clarify this with Shorty to be fully certain of this.

[snoozer]

Ahh, yeah reading it like that it makes more sense. Lesson learned: wash with NP first and then adjust pH SLOWLY!
I'll let yez know how it goes, thanks again

[snoozer]

Well it turns out it was just lye/iodide crystals. As swim diluted it down they dissolved and the solution went from a grey mess to a milky white then finally to a dark golden residue floating on top of the milky/golden water. Took a LOT of water though! Swim is relieved that is all it was...
It seems to be fairly heavily contaminated with iodides judging by the colour of the oil, so if swim wants to remove this iodide/iodine crap swim suspects he needs to: distill the freebase, collect it then add NP to the oil/water mix and then gas it thereby making the salt and filter it out. Then dissolve the salts in water, wash with NP to remove iodides then basify again and theoretically when basified again it should be much cleaner (clear or paler yellow?) Then finally redistill. Is this correct?
OR can all this be avoided because distilling the first time simply seperates the meth from all the contaminants?

[SHORTY]

Steam distilling will not remove all the contaminants but it will remove the gold color you speak of.  It doesn't really matter how much water you add if your steam distilling so long as you have a large enough flask. 

As far as smoking the oil, i beleive wareami recently tried distillation and he used the fb oil but im not 100% sure.  I have never tried smoking it but i may do so just to see what its like.  I'll let you know when i do.

As far as the fish smell, im afraid i wouldn't be able to give a good answer.  For some reason my sense of smell has become less sensitive  to the point where xylene and toluene don't even have much of an odor to me anymore.  But i never have smelled anything like fish when doing this.

[ChemoSabe]

The NP wash prior to basing works because the freebase, due to low pH, hangs with the water and doesn't follow the NP that's doing the washing. (or something quite close to that)

Once you've based up and distilled it it will readily join with NP so washing it in this way is not then practical.

But once it's combined with an NP and then converted to the HCl salt by either titration or gassing any iodine based garbage which managed to follow it through distillation (which shouldn't be a lot if any) can easily be removed with cold, dry acetone.

A good recrystallization should then remove most if not all other crap from it. If titrating, the very last of the batch you pull over might need 2 sequential recrystalliztions to get fully free from minute "klingons".

[snoozer]

Yeah chem thats what I thought, good news about the 'tone wash removing crap too.
Well that should sort it all out, I'll report back when I have bio results.

[biotechdude]

As far as the fish smell, im afraid i wouldn't be able to give a good answer.  For some reason my sense of smell has become less sensitive  to the point where xylene and toluene don't even have much of an odor to me anymore.  But i never have smelled anything like fish when doing this.

As Swix has a more virgin nose then SHORTY, and follows his post reaction workup...he can comment.

The collected distillate of meth-fb atop of mirky lye water smells strong and is a 'crowded' fishy/lye smell.  Once the lye layer is removed and the meth-fb is water washed the smell becomes 'cleaner' and more like a unique fishy cum smell.  It should also be predominantly clear.

Swix has heard people smoking base, but has not done it himself.  He wonders if the meth-fb can be 'reduced' in volume or whether it is as concentrated as it can get when it comes over as distillate.  He then assumes an eyedropper or similar would place a small volume in the pipe and then light 'er up

[ChemoSabe]

If FB smokes/vaporizes in a fishy fashion then my next realm of inquiry would require an additional test subject. If swim's buddy was performing the test himself then he'd select a stunning female to do this portion of the test with.

Would inhaling the pure freebase vapor tend to give one "fish breath" when directly afterwards performing an act such as kissing?

And this is not an absurd joke question either. I'm serious. If swim's buddy could he'd test this immediately but he's short on several of the items necessary.

reference posts

Post 352763 (missing)

(Rhodium: "Smoking theory", Stimulants)

Post 352932 (missing)

(Rhodium: "I put that "distilled" in there to make it sound ...", Stimulants)