Author Topic: What way to go.....  (Read 11315 times)

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8ball

  • Guest
What way to go.....
« on: February 21, 2004, 02:00:00 PM »
Afer an unexpected freind turning up today and creating dramas, ive had to rush to hide some things and somehow amid all confusion have mixed wash water from tolly and distilled honey up with hydrochloric and distilled for lowering ph as well as the caustic solution that came over with honey while distilling and some honey in distilled ready for evapping which had been ph to approx 6-7. once i went to continue i ended up with emulsions and all sorts of shit.

if i ph all tolly get everything below a ph of 7 to salt so it passes to distilled add all distilled to flask and take it up to a ph of 14 and distill again will i retrieve my product again.


jackhole

  • Guest
Yes
« Reply #1 on: February 21, 2004, 02:07:00 PM »
Get the pH to 3-4, it's easier that way.  And yes, any good A/B extraction and/or distillation will recover your product.  Fear not.


8ball

  • Guest
Will a small amount of tolly ...
« Reply #2 on: February 21, 2004, 02:40:00 PM »
Will a small amount of tolly matter if it ends up in there as well.


jackhole

  • Guest
Say what?
« Reply #3 on: February 21, 2004, 02:46:00 PM »
If it ends up where?  Look, if you have any combination of reaction fluid, water, polar solvent, and non-polar solvent, just basify the entire fucking mess until it locks up, stir it every half hour for several hours.  Collect the upper non-polar phase, clean it, and distill or titrate it.  And then give me some.

And I guess the only reason you'd have a mess like that would be if you suddenly had to clean up quickly and emptied everything into a single container... which could actually be a great idea depending on your situation, ya dang varment.  ::)


wareami

  • Guest
Wash....
« Reply #4 on: February 21, 2004, 05:23:00 PM »
If the pH is below 7, Tolly wash to remove the trash then rebase and extract again.
That is where the trash is coming from!


jackhole

  • Guest
Really?
« Reply #5 on: February 21, 2004, 05:54:00 PM »
Really?  I always basify to around 4 and never accumulate trash or anything like that.  There's hardly any loss during recrystallization, and I get a higher yield by acidifying it more.  But then again, I do hella long wet refluxes - pulling 2 days  :)


wareami

  • Guest
See .....
« Reply #6 on: February 21, 2004, 06:32:00 PM »
That's the trick! Don't get the trash in there to begin with!
But since SWI8B mixed all the trash back in that he washed out the first time....it should be removed again first to avoid it from coming over.
If it's too basic when the NP wash is performed on the trashy solution, the NP will pick up some gear with the trash!
Kepp it acidic and NP wash....remove the trash with NP then add fresh NP and base again and pull!


stereoIsomer

  • Guest
Does it take time for the freebase to enter NP ?
« Reply #7 on: February 22, 2004, 09:44:00 AM »
I'd not pondered this, assuming brownian motion to be working for me, but as a follow-on question to jackhole's comment, i ask...:

Does it take on the order of several hours for the freebase to enter the NP after bassification ? clearly it's an asymptotic process, but I would have guessed a fairly quick one.. ie. on the order of seconds vs. hours...

(let's assume reasonable surface-area contact of the NP and Freebase... and 25C, sealevel conditions )

thanks in advance!

jackhole

  • Guest
It bumps up the yield
« Reply #8 on: February 22, 2004, 10:53:00 AM »
Giving the phases several hours to separate ensures that all of the freebase or hydrochloride becomes isolated into its appropriate phase in the system.  While the majority of the product is isolated rather quickly, a 5-10% increase in yield can be afforded by allowing several hours, or better yet, a full day, for complete separation.  You would think it to be an instantaneous process, but for some reason, some of the molecules are more "stubborn" than the others, and time seems to be the only way they will basify into the solvent or salt out into the dilute acid.


ici_rhi

  • Guest
Another pull
« Reply #9 on: February 22, 2004, 12:40:00 PM »
Why not do more than one pull on the NP? After basing the reaction fluid, let it set until you see no more "bubbles" eluding.  Wait at least 30 minutes, preferably more if you can. This gives most of the freebase time to migrate into the NP. Decant and add fresh NP (1st pull). Add some salt (table, pickling or rock), a small amount of base and stir. You should see more freebase migrating into the NP. Again wait several minutes, even an hour, until the eluding stops. Decant (2nd pull). You may combine the two pulls. If titrating, go with jackhole and base to about 4. This should ensure a maximum yield from these 2 pulls.

Finally, pour an agressive NP such as Xylene or Toluene over the reaction fluid, then add more base. Let this sit overnight or a day or so. Any remaining product should have migrated to the NP. You should have your yield from the A/B extraction.


CharlieBigpotato

  • Guest
how about this?
« Reply #10 on: February 22, 2004, 04:55:00 PM »
i wonder if it makes sense to do the first pull in a wide, shallow pan? so the layers are extremely close and shallow, and then dump that mix into a sep funnel for easy seperation?

the time needed for the migration is about distance, no?

SHORTY

  • Guest
Why not just steam distill and have it all in
« Reply #11 on: February 22, 2004, 05:41:00 PM »
A matter of minutes.  I would bee willing to bet that no matter how good your chemistry skills are you couldn't get more freebase out of the post rxn solution than if you were to steam distill or even just distilling without the extra steam.

How much easier could it bee?  Just add a 50/50 solution of naoh to the filtered post rxn solution until the color no longer changes when more is added.  Immediately you will see your crude meth freebase sitting on top of the water which in my opinion is enough confirmation for me and no need to test the ph.  Then just connect to your steam and condenser and in less than 15 minutes you can distill up to 10g of freebase.  Without losing a drop of honey due to mechanical losses or due to imperfect lab technique.  Its nearly impossible to fuck up cause the steam does everything for ya.


stereoIsomer

  • Guest
question, method - A/B extract or Steam Distill ?
« Reply #12 on: February 23, 2004, 12:15:00 AM »
I agree, re: distillation, Shorty. In practice, swim has found that despite owning proper glassware, the distillation is seemingly difficult to achieve in a non-lab environment. I'm referrring primarily to steam distillation where a super-heater is called for once you have generated steam..

There is of course the posting about the dwarf heater- but my suggestion here would be for an experienced distiller to "distill" their relevant knowledge AND include the final finishing steps as well- so we have a single posting that is both the kit & kaboodle for steam distillation.

My question is- is either process (A/B extraction or Steam Distillation) more effective at purifying the results of the reaction ?
for instance, will small amounts of gakkk polymers or other impurities be more or less likely to follow the honey in the A/B method ? or the steam distill ?

thanks!

morpheus

  • Guest
Which one?
« Reply #13 on: February 23, 2004, 02:17:00 AM »
Swim thinks more surfactants,polymers and gakk will
come over in an a/b.
Distill!!

biotechdude

  • Guest
Post reaction steam distillation workup.
« Reply #14 on: February 23, 2004, 02:39:00 AM »
<<I agree, re: distillation, Shorty. In practice, swim has found that despite owning proper glassware, the distillation is seemingly difficult to achieve in a non-lab environment. I'm referrring primarily to steam distillation where a super-heater is called for once you have generated steam..>>

Dude, steam distilling meth does not require the use of superheated steam or fancy setups.  SHORTY uses a kettle as his steam source by memory...

Unlike pseudo, eph etc....METH-fb comes over VERY easily.  Swix just bases and gently boils the flask.  Comes over a treat...instant clear meth-fb in 10 mins.

So all u need is a flask, bend, condenser.  Circulate the condenser water using a pond pump and bucket. 

Swix does it like this.  Shortcuts and ommiting steps is possible but not recommended.

1) Reaction solution is diluted (and setup rinsed) with 1/2 volume dH20.  Boiled for a few mins to remove free iodidne (caused by HI decomposing)

2) Solution is washed 3X with dry NP (xylene)

3) Solution is raised to pH 12+ using NaOH solution until no more colour change is observed (usually milky white)

4) Solution is steam distilled (using internal or external steam).  Distillation stopped when no more oil is seen condensing.  Glassware rinsed with dH20.

5) Distillate will contain meth-fb with some cloudy water beneath.  The bottom cloudy water layer is carefully removed.

6) The meth-fb is dissolved by addition of 2X volume of dry NP (xylene). 

7) The NP/meth-fb is washed with salt water solution.  Then hot weak NaOH soltuion, then hot dH20, then cold dH20.  Last wash should be transparent.

8) Clean NP/meth-fb is gassed to precipitate the Meth HCL.  Or titrated by adding a small ammount of dH20 and slow dropwise additions of HCL acid until pH 6.

9) Crude Meth HCL is obtained by filtering and drying the gassing, or evaping the titrated water.  Ice cold acetone flashing may be necessary to dry product.

10) Meth-HCL is subjected to slow dual-solvent recrystalisation using dry alcohol (IPA or MeOH) and dry acetone.  Repeated if impurities present.

11) Dont get caught (you'll have to figure that one out...)


Bio 0_o

CharlieBigpotato

  • Guest
good write, biotek
« Reply #15 on: February 23, 2004, 04:24:00 AM »
makes good sense.
kudos

8ball

  • Guest
Whats the big deal..
« Reply #16 on: February 23, 2004, 05:15:00 AM »
I have only ever distilled, and have only ever done hypo syns. But i have tried both washing reaction fluid and not washing the reaction fluid before distilling and to be quite honest i dont think there were any benefits for either process, the meth was just as clean with either wash or no wash, so when it comes down to it i opt for the process that reduces the chance of error.
I feel that in back yard lab situations, distilling with or without external steam or with or without that wash before distilling the product is going to be the same, external steam cuts the time down ten fold, i feel that's the only advantage.


clandestine

  • Guest
oops ok
« Reply #17 on: February 23, 2004, 09:37:00 AM »
biotech when you say wash with salt water.. you mean table salt..(non ionized) right  About how much salt would one put in 500ml of dh20 prior to the wash?

Im sorry if this post is rated as UTFSE i didnt see anything speaking of measurements of how much salt to wash with per ML of water if it matters to any degree.

Also what is the reason for using salt in the water might i add.

biotechdude

  • Guest
Comments
« Reply #18 on: February 23, 2004, 10:35:00 AM »
FIRSTLY, i have to give credit to SHORTY for the majority of knowledge gained in the aforementioned post-reaction workup summary.

<<I have only ever distilled, and have only ever done hypo syns. But i have tried both washing reaction fluid and not washing the reaction fluid before distilling and to be quite honest i dont think there were any benefits for either process, the meth was just as clean with either wash or no wash, so when it comes down to it i opt for the process that reduces the chance of error.>>

8Ball i agree, a well executed hypo synth using clean psuedo will probably not benefit from the pre-distill NP wash.  HOWEVER, for those using less-than-perfect precursers and equipment; it could be of benefit.  And to be honest, once Swix has got to the point of a finished reaction (after the week of prep work)... a quick five minute wash step is the last of his worries.

<<I feel that in back yard lab situations, distilling with or without external steam or with or without that wash before distilling the product is going to be the same, external steam cuts the time down ten fold, i feel that's the only advantage.>>

Likewise, a well executed hypo reaction will see no difference. 

From

https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth.ephedrine.steam.html



<<A separation of ephedrine from the amphetamines seems possible if a steam distillation as mild as possible is used to isolate the amphetamines. Then a forced steam distillation can be used to separately collect the ephedrine.>>

HOWEVER, on the basis of removing iodo-intermediates and other derivatives, Swix uses a gentle boil (using no external steam) to bring over the greatest majority of meth.  This is because he uses plant derived alkaloids, but this would also apply to anyone using less-than-perfect pseudo.

<<biotech when you say wash with salt water.. you mean table salt..(non ionized) right  About how much salt would one put in 500ml of dh20 prior to the wash?>>

Mmmm, when one adds the first portion of water to the meth-fb/NP and SHAKES..it doesn't separate QUICKLY and some inter-mixing dynamic happens due in part to the layers clinging to the sep funnel sides. (SHORTY could prob explain this better). 

SO some non-iodised cooking (no pun intended..) rock salt is added.  Say about a tea spoon to 200mLs.  This speedens the separation of the layers and the layers and now 'DRY' and dont mix and dont cling to the sides of the sep funnel.  Its kinda hard to explain.  But in short, you want to saturate the dH2O (with salt); but you DONT want to add TOO much so it doesn't dissolve anymore.

Geez or an Elder Bee could explain why this happens better..., But Swix thinks the salt adds ionic forces which fastens (and better ensures) the migration of molecules to where they are meant to be (eg impurites in water, meth-fb in NP). 

Bio 0_o

SHORTY

  • Guest
Steam Distillation of Meth - With Diagram
« Reply #19 on: February 23, 2004, 02:03:00 PM »
I will usually add about a tablespoon of table salt after shaking the first dh20 wash.  Not all of the salt dissolves but it is drained out through the sep with no problem.  The next wash will usually seperate quickly and there will not be any dropplets on the side of the funnel.

Incidently, when adding your acid if after you shake the sides of the sep look dry with no droplets or liiquid running down then you've added enough acid.  Its not easily noticed but after you do it enough you won't even need to check the ph.  Its accurate down to the last drop of acid.

Heres how my steam distill is setup