Cleanup: Steam vs. a/b

[place]

Hey.

SWIM and steam are not best friends, so he have a question:

Will the use of steam destilliation after a rxn both give better yield and purity than a full a/b clean up? (key plunk, a/b and a recryst.) or is steam just less difficult and faster to use?

[SHORTY]

Yes, it will give higher yeild and bee cleaner than just an a/b.  Much higher in my case considering the last time i had to do an a/b due to a broken condenser, the results were terrible.  However, for those who have more experience with a/b, the yeilds would be about the same.

[wareami]

Well...most bees in my position would steer clear from this subject by adopting the "Once Bitten...Twice Shy" attitude.
But c`mon now....?%#!
This isn't your run`o the mill, average "assless chap" yer dealin with here!

It's been common knowledge for the longest time which method of extraction produces a purer product.
Rhodium has always pushed Simple Distillation or Steam Distillation over A/Bing from all I've ever read!
He'll correct me if I'm wrong here.
Provided you have 100% quantity of the expected in solution, Yield will always be solely dependant on the skill level and experience of the extracter.
If 100% is in there to begin with, it's user error or lack of skill/experience if 100% isn't retrieved. Regardless of the method of extraction.

Many bees have been deterred from incorporating distillation because of the assumption that it takes an elaborate setup to carry out this process successfully.
I know! Ibee was deterred in the beginning because of his lack of understanding and labware.
After consulting Dwarfer and Orgy(thanx bees), Ibee's confidence level was increased when told he didn't need an elaborate set-up and some of the principals were outlined.

Some may opt to go with an elaborate setup if they have the equipment.
Ibee didn't have the equipment so he made a CRUDE distilling apparatus to get his feet wet and it worked like a charm.
He will still use this set-up if he finds himself gaaked but in cases where he's not gaaked, he's still more comfortable with the old familiar A/B for obtaining the goodz!
It's faster to base, pull, acidify and evap(A/B) than it is to base, distill, pull, acidify and evap.(distill)
But in cases where gaaked anti-xtalling agents are involved, the distilling would be the likeliest course to take.

Here is a pic of a CRUDE distilling setup as used per Ibee's corner successfully!

Ibee recommends doing this properly with proper equipment but he set out at first to just prove to hmself it could be done this CRUDE way and he was satified it could bee!

And here is a link to a proper STEAM distillation unit by SHORTY that Ibee would recommend to all that are serious about STEAM distillation

Post 490581

(SHORTY: "Steam Distillation of Meth - With Diagram", Stimulants)
And I think I recall SHORTY pointing out that the STEAM part can be left out of the set-up if one wishes.
Excellent Job SHORTY!

[DrLucifer]

While swim admits that a textbook a/b, titration and re-xtal would be a *faster* route to clean meth, he is now a firm believer that the extra effort involved, is well worth it!
Swim shamelessly duplicated shorty's design layout except swim is not using an external steam source, and swim has rented out his coil condensor. Nice lil earner  
Swim really had no choice to adopt steam distillation as he was really having trouble pulling his treasure out of his rxn fluid with standard a/b extractions.
After trialing several np sovents with minor success, he gave up in search of something better, which he found in the form of steam distillation  

[SHORTY]

If you have been doing regular a/b's for a long time and have gained the skills necessary to do it without lossing much product then that way may be faster for you.

I, however, never practiced those skills cause i started distilling right after my first couple rxns thanks to placebos writeup.  Therefore, steam distillation is much faster for me. A 10g rxn can be worked up and ready to smoke in less than 30 minutes. However, if i recrystalize then it would take little longer.  I have done it (once) in 15 minutes but yeild suffered due to not allowing enough time for layers to fully seperate etc. 

How long does it take to do a regular a/b, on average?

[place]

So fast? How do you get crystals in such a speed? Still after steam distillation, you have to extract with NP and either gas or extract with HCL water, don't you?

SWIM tried to set up a simpel steam distillation under a ephedra steam distl. like VideoEditor explan´, but if he use this 1000mL flask, the stopper "pop" out because the pressure get to high. The glass stems he use is about 5-6mm Ø. He tried his 500mL flask instead, there was no problemes. Isn't that a littel weird? Anybody said that a Ø on 5-6mm was fine.

How long time does if normally takes you guys to, that say, steam distillation a 30g batch? Using "VideoEditor: Easiest Post Rxn Steam & Clean for RP/I".

@wareami: Thanks for your tolerance    The reason SWIM was doubting, was because of the massive a/b methods informations in the FAQ.

[wareami]

Pictures are worth a thousand words and Ibee is visually driven. If it can't be mentally conceptualized(pictured), there's little chance that the bee will be driven to experimentally investigate it.
Simple distillation was one of those conceptual hurdles for Ibee until he was relatively confident he could pull it off.
Breaking down the basics is what gradually leads to fuller understanding.
This link will provide some basics if you haven't seen these yet!

http://www.chem.cuhk.edu.hk/labtech/index.asp

(Found on Rhodium's Site under Multimedia)
I encourage AWE Bees to watch these videos to get all sorts of basic lab tips!
The audio is in chinese but has english captions but you can just look at the pictures if your like The Kidz  

The introduction of this CRUDE simple distillation is by no means meant to be settled on as a final set-up.
It's merely a tool that can be used until bees advance to a stage of building a proper efficient unit.
Ibee promised aztec long ago he'd post this once he worked the kinks out.
so here is a basic description of The CRUDE Simple Distillation.
He's no authority so hopefully this will generate some feedback and pointers that Ibee may be missing.
With the CRUDE setup pictured above, just use a glass tube through the stopper connected to aquarium tubing. Ibee used a 4inch glass tube protruding into the stopper then connected aquarium tubing to it at the exit point of the flask
Don't let the glass tube protrude down near the liquid being distilled. Set UP as pictured and it will work fine.
Never fill the distilling flask past the 2/3 mark.
Post-rxn filter to get the honey.
Add dh2o to dilute some.
Base to pH13-15
Cap off with stopper/tubing and set flask into oilbath.
Run tubing into receiving flask.
Ibee cranks his wok up to 350°F
A steady rolling boil is what is looked for and then the FB will start coming over along with some waste water.
After all the oil is collected, separate the water and put back into distilling flask as it will still have some residual M molecules.
Wash the oil with clean h2o and put the wash water into the distilling flask for the same reason as above.
Add NP to the oil to pull the oil then titrate the NP with dh2o and hcl.
There ya have it!
CRUDE and Simple!

[Osmium]

> Post-rxn filter to get the honey.
> Add dh2o to dilute some.
> Base to pH13-15

Why don't you steam distill for a few minutes before you basify? This will remove more crap.

[Organikum]

Dont know if it was already mentioned here.
You can steamdistill directly into diluted HCl (10%), evap, acetone wash to remove excess acid and - and actually this should be followed by an recrystallization but I know, I know......

But if done this way or if the last step is titration - it is piggystyle to use MURIATIC acid from Home-Depot or similar as this stuff is DIRTY like hell. Distilling into HCl or titration has to be done with distilled HCl or labgrade HCl (so acessible).

thats my opinion of course, nothing more.

EDIT: Osmium is absolutely right here. Boil the shit some time with water added in the open vessel before basifying and steaming - this will remove gakk which goes through the reaction and also comes over with steam.

[SHORTY]

So fast? How do you get crystals in such a speed? Still after steam distillation, you have to extract with NP and either gas or extract with HCL water, don't you?


I steam distill into my sep funnel and then drain out the water and add toluene.  Wash the tol with dh20 and then with salt water and again with dh20.  I then add more dh20 and hcl and drain into a visionware saucepan.  I then gently heat until almost dry and flash with acetone and decant the acetone.  The visionware stays warm and the crystals dry out in about 5 minutes.

[Smilaxium]

In SWIMS experience, the amount of free base you have to work up is directing which way to go. When steam distilling small quantities of freebase (< 100 ml) SWIM always has a lousy 50-60% recovery. There is still a reasonable amount of freebase in the water layer (extract with NP solvent before throwing away!) and within the distillation set-up. However, for larger amounts (500-1000 mls) steam distillation is becoming more attractive. Relatively, you will loose less free base and the overall yields are higher.

[wareami]

>Why don't you steam distill for a few minutes before you basify? This will remove more crap.

Okay Os...Okay....I can feel the undertow of the "Universal Syntax Pool" pulling me into verbal grammatical submission.
How was I suppose to know that STEAM distillation doesn't always require an External STEAM source?
Thanx Os...
Never considered that step but it makes perfect sense and will be included from here on.
Orgy: Ibee tried that distilling into dilute hcl, but it was only once and received poor results and now that he thinks back, he said that it was tried during the time he learned about over filling the flask.
Alot of NAOH crapwater distilled over and everything smoked like a barbie Q.
He scratched his head, then upon realizing what was happening, he said "Never do that again"!
He got nothing but salt back for that blunder!
Next time he'll try your suggestion the right way.
Thanx Dewd!

In all actuality, with all things considered, steam distilling is the fastest route because during A/B, several pulls are done whereas in SD`ing everything comes over at once.
About the A/B faster statement, Ibee was speaking more from that "instant gratification" mindset of getting a motivational blast in the time it takes to evap 20ml off the first pull.
And shorty is absolutely right in his observations about A/B`ing compared to steam distillation.
It takes alot of practice to get good enough to pull "AWE" everytime doing an A/B.
Bees also need to consider that most of Ibees runs are nano because of all the pfed extraction experimentation.
He's not a big batch bee! But if he were, he'd steam distill everytime without question.

[SHORTY]

As far as the water layer holding meth, i have evapped the water layer a few times and as far as i could tell there wasn't anything worth keeping left.  There probaly is some but i find it hard to beleive that 50% - 60% was caused by distilling a nano. How could there bee such a drop in yeild just because a small amount was distilled?  It would bee nearly impossible to lose a considerable amount due to mechanical losses when steam distilling.  As long as you have added sufficient base then all the freebase meth will come over and then if allowed to continue the steam will clean the setup by pushing any residue fb in the tubing to the condenser which can then be rinsed to flush any residue in it to the receiving vessel.  Also when doing a small amount if you use a sep funnel as a receiver then it is much easier to see how much fb you have as opposed to a flask or beaker.

[wareami]

Shorty's observations mimic Ibee's.
It may have been noticed that over the past two years, there's been a pH shift when working UP the rxns from OTC pills.
When Ibee started out, it would take half the amount of NAOH to base than it does nowadaze.
The underlyeing cause is anybees guess!
Ibee just learned to deal with it and when yields were very low compared to the expected after a full reduction, he always knew to base the hell out the post-rxn to claim the rest during a/b.
Ibee became obsessed with yield because most reported lower yields than Ibee would recover and record.
Alot of those descrepancies were found to be the result of LWR compared to most at the time still doing p/p hot and fast.
But Ibee wasn't convinced that that was the sole reason.
Ibee would suggest to others to GO back and base the hell out it when they reported losses and the bees would come back and report successful recovery of some.
This led Ibee to believe that most of those losses were due to pH adjustment problems in most cases.
Since Ibee has been a nano bee...Walking away from a work-up with less than 85% just wouldn't bee worth AWE the time and effort he poured into the rxn.
That was just his take and he kept at it until that became the norm for him.
Keep in mind...this wasn't overnite success.
A good year of practice went into the refinement of technique employing every conceivable combo in A/B`ing.
To hear him tell it, he's still no master a/b`er but the #'s aint too shabby cause he wouldn't ever settle for less!
Dogged determination and perfectionism make for strange bedfellows! Marry the two and yer in for a deadly accurate ride if you can get past AWE the frustration!
The LWR coming down the pike when it did just tacked on a few % to the expected which outweighed "instant gratification" tenfold!
It also kicked Ibee into the twilight zone ashamed to report his yields for fear he'd be christened a liarbee!
Steam Distilling or A/B`ing....when in doubt...base it out!

[biotechdude]

As just about every point has been covered well, Swix will add another small comment

Steam distilling is a great way to isolate the meth from the reaction at ~95% purity.

Then it is a good idea to clean the isolated meth by doing an A/B.  This is done by adding NP to the freebase distillate, and proceeding with different washes; until finishing by converting to the hcl salt.  This produces your relative ~100% purity.

So rather than say - "this is better than that"

Its apparent that both have their merits and should be teamed together for best results; and finishing all proceedings with a recrystalisation.

[Grignard]

Steam destillation only takes about 2 hour in a 30g batch and you dont need anything else than the flask you use for your buchner funnel.. plug the sidearm and put a stopper in the top vith a hose and conect this to the round bottom side arm with glass tubing to the bottom.. This is very fast to do and you get high yeld.. Then seperate the water and put in some toluene.. I use to do a fast a/b to remove some of the yellow colour and titrate out the meth vith 10% HCl.. But the evaporation takes a while.. then i wash with acetone to get rid of some HCl. Dont hurry, if you stressing in the workup you will lose yield..  

[SHORTY]

Why so long?  Even without external steam it has never taken me that long.

Biotechdude's procedure is the one i follow and in my opinion is the quickest, cleanest route to follow.