Author Topic: The post-reaction workup: a cook's summary  (Read 10298 times)

0 Members and 1 Guest are viewing this topic.

swEEt_tooth

  • Guest
Does size matter?
« Reply #20 on: April 23, 2003, 04:13:00 AM »

a_mean_bee

  • Guest
re: does size matter?
« Reply #21 on: April 23, 2003, 04:48:00 AM »
you're trolling with that post, right? Hoping for a flame, maybe.

Considering everything that the write-up touches on it's not that long. I'd guess that the target audience would be relatively novice. People who perhaps don't already know everything.


ballzofsteel

  • Guest
Why question its relevance with such originality?
« Reply #22 on: April 23, 2003, 04:54:00 AM »
I dont see how,that with all of the simple explanations posted out there,so many questions go un-answers,and so many need be countlessly re-hashed.

This post covers indepth,from a-b all of these possible questions,
and pretty much makes redundant about 1/4 of all postings Ive read on this forum.Why nock it?

So we have the step by step extraxtion protocol,the post rxn work up,the a/b,the stims FAQ,all Geez has to do now is document every variable to every rxn,and we can close the book on this forum for good. :P
Get cracking Geez,I need this by friday if possible.

Thankyou in advance ;)

Ballz

halfkast

  • Guest
Geez! what have ya got here for us??!
« Reply #23 on: April 23, 2003, 07:41:00 AM »
Geez! what have ya got here for us??!
That was bloody excellent just what I always wanted, a respectable text on post reaction work. :-[

Organikum

  • Guest
just ignore ChesterCopperpot aka swEEt_tooth
« Reply #24 on: April 23, 2003, 09:31:00 AM »
He is a resident low level troll (LLT) in pre-ban status. And he is loosing rapid on quality in trolling. Copying Osmium. A troll trolls by copying a moderator. buhahahah.....
Disgusting.


SQUIDIPPY

  • Guest
reply
« Reply #25 on: April 23, 2003, 12:31:00 PM »
Excellent write-up geez! Complete, and comprehensive.

S/D how ever , (all though he finds it hard to believe), in a way, must agree with Osmium, that it is a fairly basic operation, that somehow takes on the appearance of the complex. So S/D is going to offer his slipstream “ghetto”  post RNX workup.

Many bees, especially newbees, don’t have access or the money for lab equipment. Weather due to a limited time window, or whatever reason, often the trade off of time for a few percentage’s of yield is a desirable one.
S/D has spent many years, finding the best balance between time and effectiveness. The following is the result.


You will need

1 pint size jar with water tight lid
1 quart size jar
1 Pyrex beaker (pref 1000 ml. But any size will do)
1 turkey baster
1 stirring rod, (preferably glass), but clean un-finished wood will do.
RDL
Ice Cubes, (4-8)
Salt
Coffee filter and funnel


Fill you beaker with 100ml of H20, sprinkle in some RDL, slowly and stir. Feel the beaker bottom with your hand, continue to add RDL until it heats up real nice. This is not critical so don’t sweat it. Place this off to the side for now.

Bring contents of flask to a rolling boil a few minutes. Remove from heat and let stand until settled. Hold it up in the light. What do you see?

Liquid is;
Clear = Excellent, that’s what you’re looking for.

Cloudy (slight milky color)= You should be ok, yield might be low, you didn’t do a good job of filtering when you extracted.

Light yellow= Some gak was still in your pfed, yield and quality, will most likely be low. Extracting technique needs some work.

Dark yellow or any orange color= return to heat and boil for a few more minutes. Any excess Iodine will boil off. A splash of Acetone can be added here, taking care that the liquid has cooled a bit, as the Acetone will boil upon contact, if the solution is too hot.

Now if it’s still orange, you’ve been Gaked, you may get some low quality product, you may get some pfed, you may get nothing. Work on your extraction technique.


Pour 400 or 500ml n/p of your choice(S/D prefers Xylene)  into quart size jar. Drop in a handful(4 or 5), ice cubes. On top place your funnel with three coffee filters. Make sure you pre wet the filters with some water.
Now slowly pour the liquid into the filter. Add more h2o to your flask and again bring to a boil, (microwave is the desired option). Observe the action, the R/P should rise to the surface of the H20, as it heats and then sink as it boils, this means that your R/P in clean.
Pour  through filter, add H20 and repeat the last step. This time dump the entire contents into the filter. Add some H20 to completely rinse out the flask. Gently squeeze and twist the filter closed. When this is dry, be sure and save the top filter. As Geez mentioned, the fine R/P will coat the filter. That problem can bee remedy by simply saving the top filter and reusing it as the top filter. This can bee done five or six times before it needs replaced.

Now slowly pour in some of your RDL mix, and stir rapidly. Observe! We’re looking for the bubbles from the top and bottom, to come together at the same speed, and the liquid at the bottom to get slightly thick. This is something that just takes practice to get the look and feel for. Best rule is if in doubt add some more RDL mix. Feel the jar during this operation, if it gets more than slightly warm, then add a few more ice cubes.
Now add some salt. Don’t bee afraid, dump some in, a half a cup. Stir and add salt until no more can bee absorbed by the liquid, and excess salt stands on the bottom. Now stir rapidly and observe. Do you see a million little bubble rushing to the top? Good! Is the top and bottom of the bubbled closing in at the same rate? Good! If you have a large amount of emulsions a bit of Acetone sometimes will help.

Now, fill your beaker up with solution. Using the pourer on your beaker, carefully pour off the xylene, into the pint jar.Take an empty solvent can and pour into it the water/lye . This will bee our emergency jug, of which once it’s full we can tap for a few G’s. Continue until all of your liquid has been separated and your Xylene is in one jar. Now fill with equal volume of cold H20, screw on watertight lid and shake. Remove lid and with your turkey baster, suck out the bottom(water), layer. Newbees, should save this layer.
Repeat the wash again only this time use warm H20.
Repeat a third time with cold H20.
Make sure all H20 is removed,  and titrate, or heat and gas.

There you are folks, simple easy, quick, and less than 1,000 words.
S/D posted this because, there’s an old saying, It goes;

A man with one watch, always knows what time it is.
A man with two, is never sure.
:)  ::)
                             -S/D


ol8dbee

  • Guest
Wish I had this write-up sooner...but
« Reply #26 on: April 23, 2003, 01:28:00 PM »
Wish I had this write up sooner, but much better late than never. As I'm sure most will agree with, as does Geeze himself, most of this info was already written up somewhere in TFSE, BUT the countless hours pouring over the stuff and the ensuing confusion when minor dissagreements occurred, was very difficult, especially if one was/is new to the honeymaking trade and chemically challenged at that.  Therefore, thank you, thank you, thank you.  xxx's & ooo's
ol8d.

WizardX

  • Guest
Well done!
« Reply #27 on: April 23, 2003, 02:23:00 PM »
geezmeister: All I can say is nice work and keep it up.

Osmium

  • Guest
RP/I2 post-reaction workup: The short version
« Reply #28 on: April 23, 2003, 04:52:00 PM »
*almost speechless*

Almost, but not totally.

Once you're done with the reflux let it cool down a little (or don't, doesn't really matter). Colour doesn't matter either, mine was always almost black due to I2. Dilute with several volumes of water, because pouring conc. HI through filter paper is a pretty dumb idea, and concentrated solutions aren't easily extracted. Just fill up that flask with water, suction filter out the rP, rinse flask once or twice more with water and pour it through the same filter too. Use proper lab grade filter paper and you will catch all rP during the first time.
The dilution with all that water will cause the non-acid soluble side products to come out of solution. The shit turns yellowish/reddish and milky. You cannot look through it easily anymore.
To remove the unwanted shit rinse the flask with some NP solvent (toluene and xylene being prefered). Pour through the same filter still holding the rP. Shake the shit out of the NP/water layer, because half-assed stirring isn't good enough. Let phases separate, discard NP layer. Repeat NP wash twice. Most of the colour and pretty much all of the side-products will be gone by now.
Evap the NP washes if you like, so you can look at that nasty gunk this simple step removes.
Wash the rP with a little acetone or MeOH, let it dry and reuse it.

Basify the strongly acidic water layer with NaOH solution. Concentration doesn't matter, 20% should be ok. pH doesn't matter either as long as it's strongly basic. Nothing wrong with pH14 at this point. The solution will heat up considerably, and the meth freebase can be seen. Extract it a few times with tolly. Shake hard. Take your time, let layers separate completely. The water layer might start to solidify into a slush while it cools down. Do not freak out. There's a whole lot of sodium phosphate and sodium iodide in there. Simply add some hot water to redissolve everything, and proceed.

Then gas the tolly solution. If you were careful when separating the layers you don't even need to dry the tolly prior to gassing.
Filter out the product, barely cover the product with acetone, suck dry (just add the acetone to the tolly containing your freebase), repeat gassing until nothing comes out anymore. I've had reactions where I had to interrupt the gassing 8 or 9 times to filter out the product.

Optional, often not needed: dissolve already bright white meth dust produced that way in a little hot anhydrous IPA. Add several volumes of acetone. Place in freezer overnight. Filter out product. Solvents from gassing and this recrystallisation are combined, evaporated (*), and the residue is again dissolved in a little hot IPA. Gas the IPA with HCl to make sure all meth is neutralized, add excess of acetone, into freezer for a few hours, filter out additional crop of product. Evap solvents just for shit and giggles, and tweak around with it for an afternoon or two, maybe you will get another line of mmmmeth out of it. Or just dump that shit. Or save it to be worked up some future time.

(*)If you have a rotovap you can easily separate the solvents at this stage and reuse them. The tolly for example can be used to wash the still acidic post reaction mixture. IPA/acetone is used to rinse flasks and glassware. A rotovap will speed all this up considerably, and you can e.g isolate the meth freebase before crystallisation by removing all sovents under vacuum.


FINALLY:

The short version:
dilute with plenty of water, filter rP out, extract the crap with NP (3 times, discard), basify the water layer, extract freebase into tolly (3,4 times is ok), gas it. Recrystallise product. Done.

Look! Two lines, and all is said!

You drama kings make this shit way too complicated.
Never judge a reaction by its looks, colour or whatever. You won't know until you're finished, and all this drama will only wreck your nerves.


geezmeister

  • Guest
The second round of bets
« Reply #29 on: April 23, 2003, 06:16:00 PM »
Oooh oooh ooooh! Thanks. I won the second round of bets, too! I bet the paycheck it would be longer than ten lines.
Pay off boys!

Oh... Thanks, Os! ;)  

(I'll put your cut in the mail tomorrow.)


Osmium

  • Guest
Saving solvents: Countercurrent extraction/washing
« Reply #30 on: April 23, 2003, 06:56:00 PM »
The 20 lines were just some minor warming up. The actual procedure description is only two lines.

Forgot to add: no need to neutralise the residual I2, the NP washes and NaOH will take care of the minor amounts that might still be present.
Also, don't go overboard with the amount of NP solvents during the washes. Rather use less and wash once more, and when processing bigger batches you can further save on organic solvents by dividing up the post reaction mixture to be processed into several containers A, B, C.
Extract A with NP solvent. Discard it (or use it on B and C if you want). Then use the same amount of new solvent to wash the acidic post reaction mix in container A, and when done transfer it to B to be used as the first washing/extraction of container B; the third extraction from container A is then used for the second extraction of container B and then the first extraction of container C, and then discarded. For the third extraction of container B new solvent would then be used, and that will then be poured into C for the second extraction of that water layer. And so on...
Was that too complicated? Make a drawing and you will figure it out, think countercurrent extraction/washing and it should become clearer.


SHORTY

  • Guest
Yeah if your a chemist
« Reply #31 on: April 23, 2003, 07:01:00 PM »
Yeah that could easily bee followed if you are a chemist or have been hanging around the hive for a couple years.  However, i doubt that most bees who vistit the stim forum are not chemist.  Most of us already have our own professions.  Therefore, the write-up by geez provides all the info needed by a Non-Chemist to successfully complete the synth.  Geez didn't have to do write that post and gets nothing for it other than gratification.

It seems that since no bee can find anything incorrect in his post that now its being critized for the length of it?


johndee

  • Guest
A short note from SwiJD
« Reply #32 on: April 23, 2003, 07:12:00 PM »
"And bees, if you get bored with gassing and filtering, just gas til you feel the solution is at optimum for crystallization - usually a full third of your crop of crystals from tol will not form immediately, but will coalesce and grow more slowly, and more dense. We can take advantage of that. ;D

But first as an experiment gas one til it gels and the crystals stop rolling around as soon as the wand is lifted from the medium. Get yourself a nice "slushy"!

And now just cover that nice heavy glass container of solvent and gelifying crystals and put that baby in a freezer. Come back in ten or twelve hours and pour off the solvent through a filter, now check the interior of the vessel! Still mushy so set it somewhere cold to dry, like right in the fan current of the refrigerator, or freezer - Ok now leave for another twelve hours or so. Come back with a filter and a little acetone and and maybe an icepick. and harvest superdense and clear "Ice". An order of magnitude more potent and pleasant! (when it is REAL, like this will bee, and not simulated with MSM!) Known symptoms of overuse include dependence, priapism, (grab your significant other and lock the house up for marathon sex!) confusion, extreme paranoia - Good Fun!  8)  Hey, slow down, no kidding, bee careful with that!" :o


a_mean_bee

  • Guest
addendums now?
« Reply #33 on: April 23, 2003, 07:49:00 PM »

SQUIDIPPY

  • Guest
blanketed
« Reply #34 on: April 24, 2003, 05:38:00 AM »
If this thread did not cover every possible aspect, from every possible prospective, of the post RNX, someone please add it. It appears that this subject has been blanketed.

                                              -S/D


platcat

  • Guest
X variable
« Reply #35 on: April 24, 2003, 05:46:00 AM »

SHORTY

  • Guest
This was what i meant to say
« Reply #36 on: April 24, 2003, 03:49:00 PM »
Actually Geez has done us all a favor by taking the time to do this writeup.  Redundant questions will be greatly reduced and newbees will be kept busy learning the skills rather than asking how, why, when and what. 

Those who chose chemistry as their profession and have had a formal education will tell us that this is all learned in the first few months of college or even in high school.  I do not doubt that one bit.  However, many of us had to learn the hardway.  There is a big difference between learning from a qualified teacher and learning from the internet.  Those who had the teacher often fail to realize how complicated things like basing and gassing etc... can be to someone who has never heard these terms used. 

Teachers follow a curriculum which is put together in such a way that the student will be able to gradually learn the basics up to the advanced topics.  Without a curriculum it is a much longer, bumpier, road which leads to the full understanding of the particular subject. 

For example, pick a subject which you would really like to learn about but have not had any former education on.  Now, instead of a teacher you are shown to a room which has stacks of data on the subject you would like to learn.   However, you are told that although it is organized, some of what you find will be 100% accurate and some will be 100% wrong.  Most of it will be somewhere in between.   So unlike a textbook that a teacher would provide, you cannot assume that anything you read will be accurate or not.  The only way to know is to test it yourself. 

So you set off on your journey to learn all about this subject that you want understand so badly.  Along the way you get excited, disappointed, angry, frustrated, happy, relieved.   You sometimes take a wrong turn and end up losing alot of time, money and for some, freedom. 

Also, along the way you come across certain names which stick out in your mind, some for being accurate some for being bullshitters.  One day as you continue on your journey you come across a writeup which details everything from a to z on the subject which you have been working so hard to learn.  Not only that, but it is written by one of those names which stick out in your mind as being a source of good, accurate information.  Now all the answers you have been working so hard to find are all right here in one place and there is not a doubt in your mind that what is written is 100% accurate.  I am sure that feeling was felt many times over after this thread was released.

Geez has helped me several times and has never left an email unanswered and i am sure he has done the same for many more.  How he is able to maintain his composure is beyond me.  His tolerance for such unwarranted criticism is amazing. 

Osmium,

Geez has never put you down and as a matter of fact he has backed you up on several occasions.  Yet, you criticize him for no reason whatsoever.  Just remember if it weren’t for people like Geez, odds are you wouldn't know anything either.  It certainly took a person with his qualities to put up with a student like you.  I know that this will mean nothing to you but I don't care.  Someone had to say it.


geezmeister

  • Guest
Whoa! And a question of OS
« Reply #37 on: April 24, 2003, 05:24:00 PM »
Whoa! I don't consider Osmium's comments as being critical. They're just Osmium's comments. He can't help it if the chemistry igonorant among us appear to him to be just that. We are. So what?

He made some interesting points in his narrative, as did Squidippy. I learned something from each of them in the exhange. (If I can remember what it was, at least. Otherwise it just goes down as "education"-- i.e. what's left after you forget what you learned.) That's what this place is about. (No, not the "forgetting" part.) If Os can't have some fun with us, what's the point in modding this forum, for chrissakes?

Hell, if nothing else it goaded a few extra tips out of him. In another month or so someone will likely explain them in a way some chemistry illiterate fellow might understand. You never know, even a lawyer might get it. (I doubt it though, they're pretty dense.)

Question to OS:

You advise diluting more immediately post-reaction than I am familiar with, then washing with non-polar solvent and shaking. The additional volume of water used to dilute is, as I understand your narrative, useful in removing crap that would otherwise remain in an acidic solution. (I accept this as another one of those small things I would have known if I had ever taken Chemistry. As I recall the girls who took Physics all seemed to have bigger...er, ... um, never mind.)

Later you advise that while extracting the freebase meth with nonpolar solvent you shake the solution and nonpolar solvent. Perhaps with the added water and cleaning at the first, but without, I'd strenuously advise against this. You likely are familiar with solutions a great deal cleaner than the clandestine cook achieves, or perhaps your washing technique is far superior to ours. The shaking that you advise will give the average cook an emulsion from hell that will not go away for hours and hours, if then. BTDT. I only make the comment to keep someone with a less than clean solution from falling into this problem. There are countless posts from cooks, rather than chemists, about "emulsion Hell."

I plan to use the additional water dilution at the first to see how this impacts the potential for emulsions during extracting. I imagine you will, as usual, be found to be correct.

And--- thanks for the information (you wordy chemist, you!) ;)


SQUIDIPPY

  • Guest
Good points
« Reply #38 on: April 25, 2003, 12:00:00 AM »
The points that Shorty bring up are good ones. S/D wasnt's to say that all newbees are extremely lucky to have the Hive. When S/D learned there, was no hive. He had to gather info piece by piece, attempt to sort out the good from the bad, and then trial and error his way through it. It took him the better part of a year and a half. He would have been overjoyed to have a reference site such as the hive. On many occasions, he sat, hands on his head, almost in tears, staring at a jar of liquid, of which he had piled hundreds of dollers into and had yielded nothing. Many times he thought, "If only there were someone that I could ask"


Geez, are you refering to adding H20, to the post RNX? S/D usually ads two or three times the volume H20 to his post RNX mix and then boils for a few minutes.


Os, did S/D understand correctly, that you said to add Acetone to your N/P, and then gassing?

                           -S/D


barkingburro

  • Guest
a tip i just learned
« Reply #39 on: April 25, 2003, 02:51:00 AM »
grind up some activated charcoal. about a small button sized pile and dump it into your solution. the charcoal acts like a polar solvent as is my understanding. have not tried yet but here is the write up :

activated charcoal is ultrafinely dicided carbon with lots of places for big huge polar impurity molecules to go. if you use too much however it will ALSO suck up your product. and if your product should be clear, white or lightly colored the charcoal will add a grey tint if too much is used. sometimes the impurities will be of a nature to be unfazed by the charcoal and it will only suck in product. it can be a very trial and error method, but if used correctly will greatly improve the time to purify as well as the levels of purity.

1. remove flask of filthy product from heat and swirl, ensuring an even level of heat throughout mixture.
2. add about a pea sized clump of activated charcoal. stir and heat. the solution should look black before stirring.
3. filter off carbon and impurites. watch for any product that may have been attracted to the carbon. once filtration has completed wash this product off the carbon with the heated solvent used in your solution.
4. you are done. freshly filtered mixture should now be loads cleaner than previously but may need another application of charcoal. if too much charcoal was used and the mix is grey, another wash with charcoal is needed, but should be done with less carbon. this wash can also be done with undissolved crystals to further remove impurites and is especially useful for purifying very small crystals.

i will be trying this tonite. cheers