Crystallization Question

[icecream_man]

I have two questions on the following Crystallization Process... could someone answer them for me I would apppreicate it.

Crystallization Process:

Add 8 grams lye to a clean test tube. Now add 20 ml of dh20 and mix well (use gloves if you shake tube using your finger as a stopper!) then place in sand to cool.

Add 50 ml lighter fluid to your yellow liquid. When cool add lye solution SLOWLY to the tube with the yellow liquid and lighter fluid. Don't pour in all at once, add splashes until gone. Cover the hole and give it one good shake, release the pressure and place in the sand for approx 15 minutes. Your lye will be locked on the bottom which is fine. Pour off lighter fluid into a clean test tube. Add 20 mls Dh20, 4 drops of acid and shake hard,

(Question one pertains to that last step. Am I adding the Dh2o to the acid to the lighter fluid or what was left after I poured off the lighter fluid)

Use an eyedropper to get the bottom layer, attaching aquarium vacuum tubing to extend the length if needed. Pour this into a glass dish and evaporate.

(here is the second question: Am I pouring what i got out of the bottom with the aquarium tubing or am I pouring out what was left in the tube after getting the bottom layer)

What remains after Dh20 evaporates is pure meth. Scrape crystals w/ razor and enjoy! Thats all folks.

I am sorry to be asking jhust dumb questions. My first posting was reguarding some questions on a 100 gram recipe which btw gave many of my friends a happy new year. However I really am not comfortable having a lot of shit laying around the house and would like to hypathetically jkust be able to produce a gram or two a week for my own personal use :-)  Thanks in advance for any help. :-)~~~

[biotechdude]

1) Have rxn solution
2) Add NP
3) shake and remove NP
4) Add NP again
5) Add NaOH solution slowly
6) Shake and remove NP (may want to do 2nd NP pull from based rxn solution)
7) Add water to NP/meth-fb
Shake and remove water (could also wash with NaOH solution and/or hot/cold water washes)
9) Add water again to NP/meth-fb
10) Add HCL solution dropwise until ~pH6
11) Remove water layer which has meth-hcl in it
12) Evap meth water on low heat using fan
13) Recrystalise if wanted using hot solvent slowly cooled

Depending on the purity of your feedstock; more or less post reaction cleaning steps may be needed.  Do it all in the one tube; and use syringes/extender tubing to make separations.

This was written in about 1 min...

[pyroflatus]

" Pour off lighter fluid into a clean test tube. Add 20 mls Dh20, 4 drops of acid and shake hard,"

(Question one pertains to that last step. Am I adding the Dh2o to the acid to the lighter fluid or what was left after I poured off the lighter fluid)

Apparently you add 20mL of water to the test tube continaing the lighter fluid (your non polar solvent) and then add four drops of acid to the same test tube. This is the acidification step of an AB extraction, and upon addition, your product will leave the non polar layer (the lighter fluid) and enter the water layer (as a hydrochloride salt).

"Use an eyedropper to get the bottom layer, attaching aquarium vacuum tubing to extend the length if needed. Pour this into a glass dish and evaporate."

(here is the second question: Am I pouring what i got out of the bottom with the aquarium tubing or am I pouring out what was left in the tube after getting the bottom layer)
You are pouring the lower layer that you removed with the eyedropper (the aqueous layer containing the product as a hydrochloride salt) onto a glass dish and evaporating it.

[CharlieBigpotato]

this sounds like curbshot's absurd nano rxn.
much as i liked the guy, its a fairly wanky rxn post.
for one thing, the notion that what one is left with is "pure meth" is downright laughable.
also, what's the point of locking up the np w/ lye?
how can molecules migrate effectively in a wad of soap?

also, how can a bee have such questions if he claims to have already had big success w/ large amts?

oh well
glad i ain't dreaming this dream

[icecream_man]

no claimed to any great success. It's amazing the attitude one gets here. I am capable of following directions. I followed the directions on a 100gm recipe and when I had questions I asked got the answer and finished with success. I can also make biscuits from scratch by following directions doesn't mean I know the chemistry as to why the final product comes out perfect. I pray I never have the holier than thou attitude that I have seen here.

[ChemoSabe]

This is the basis upon which the entirety my (theoretical of course) knowledge of chemistry all sprouted outwards from.

In that regard I'll always in some way hold curbshot as some sort of mythical figure.

Granted, it is a crude and caveman-like recipe but it does contain the essential and core reaction basics in a form that can be easily comprehended and executed by a relative dim-wit.

Although due to a few newer iterations of supergakks I would doubt that one could now come anywhere close to ending up with the "fat bowl" that the author claims you'll be left with to smoke at the end of it.

More relevant would be if someone were now to publish something in the ballpark of a "long wet reflux for dummies".

[Osmium]

> Granted, it is a crude and caveman-like recipe but it does
> contain the essential and core reaction basics in a form that
> can be easily comprehended and executed by a relative dim-wit.

It might contain the essential and core reaction basics that are easily comprehended for chili, but unfortunately not for meth.

> More relevant would be if someone were now to publish something
> in the ballpark of a "long wet reflux for dummies".

It has been posted repeatedly, but it probably was overlooked by most people since it wasn't at least 3 pages long when printed out and didn't contain all the extremely funny and mystical puns and jokes and typos and shit.
Too bad that the signal to noise ratio is the way it is in this forum, and that even the most sophisticated bullshit filters get clogged so fast in here.

[ChemoSabe]

Osmium osmotically stated...

It has been posted repeatedly, but it probably was overlooked by most people since it wasn't at least 3 pages long when printed out and didn't contain all the extremely funny and mystical puns and jokes and typos and shit.

let me rephrase that then

More relevant would be if someone were now to publish a "hit single" version of the "long wet reflux for dummies".

Curbshot was able to retire and then pay cash for a beachfront mansion, a large yacht and a few live-in lovin' maids with the royalties he got from just that one post.

[Osmium]

Which proves that people will only believe what they want to hear. Fuck facts and science and shit, garage cooks need none of that scientific hoopla to cook chili!

[SHORTY]

Materials

•   10g Pseudoephedrine Hydrochloride
•   10g Red Phosphorous
•   15g Iodine
•   8ml Dh20
•   250ml Erlenmeyer Flask
•   Heat Source
•   Condenser
•   Balloon


Procedure

•   Add rp and dh20 to the flask. Divide iodine into 4 portions and add each portion swirling between additions.

•   Next add pseudo and attach condenser with balloon secured to the end.

•   Slowly heat the flask to 100C give or take 10C.

•   Allow to reflux for 36-48 hours.

•   Add equal amount of dh20 and filter rp out.


Acid/Base Extraction

•   Wash filtered solution with np.

•   Add 50/50 solution of Naoh slowly until there is no color change when more is added

•   Steam distill or add np to collect freebase meth.

•   Wash np with dh20 3 times or until both are fairly clear.

•   Titrate or gas with hcl to obtain methamphetamine hydrochloride.


Recrystalization

•   Put meth in flask and cover with about an inch of acetone.

•   Bring acetone to boil on hotplate.

•   Slowly add alcohol to boiling acetone until all solids dissolve.

•   Remove from heat and stopper the flask.

•   Allow to cool to room temp undisturbed for at least 1 hour.

•   Place in ref for at least 1hour.

•   Place in freezer for at least 1 hour.

•   Filter out crystals.

•   Pour fresh, dry acetone over crystals 2 times.

•   Allow to dry.

[icecream_man]

Thanks for posting this wet long reflux recipe. It's through and makes sense. It's clear and to the point almost like a recipe for making a cake. I do have a couple questions and would appreicate the answers.

1st from Acid/Base Reaction
after putting the lye/Dh2o stop I would prefer to all np to collect the meth. Here is my question:

When I put the np in the Naoh/reaction fluid i add it in swirling it around to collect the meth. the meth would leave the reaction fluid and go into the np. I would then remove the top layer which would be the np/meth. I know that isn't exactly a question but that is correct right?

• Wash np with dh20 3 times or until both are fairly clear.
Now this is the question. The meth is now in the NP. What is the procedure to wash a np/meth with Dh20. You have two liquids one heavier than the other. How does one wash the other?

I just wanted to make sure i had those two things down before hypathetically attempting this procedure.

Also what can of yeild could one expect?

[ChemoSabe]

The guy driving the ice cream truck axed Also what can of yeild could one expect?

For newbees I'd divide the starting amount by 3 to get the total yeild for recrystallized goods. Meaning that if you really expect to end up with 10g's of recrystallized then start with a 30g batch. And expect to get around an 8ball from starting with 10g's.

This should go up as your lab technique improves.

[SHORTY]

Yes the np will collect the meth freebase as long as the rxn solution is strongly basic.

Washing is normally done in a sep funnel and consist of adding water to the np, shaking and draining the bottom water layer, (some nps like chloroform will form the bottom layer rather than top but tol, xylene, naptha will bee on top).

As far as yeilds are concerned, i havent done a rp synth for quite a while so i can't answer that question.