Author Topic: How much NP?  (Read 2558 times)

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killerbeezzz

  • Guest
How much NP?
« on: October 20, 2004, 11:02:00 PM »
Swim UTFSE looking for the ratio of freebase to non polar solvent to use when gassing.  There does not seem to be any concesis on this topid.  He Has seen any were from 8 to 1 or even 4to1 .  Also are you supposed to gas slowly or just let her rip?  Any gassing tips would be great.

jackhole

  • Guest
4 to 1 is fine
« Reply #1 on: October 21, 2004, 12:07:00 AM »
4 parts solvent to 1 part base is fine. But don't go below it. And make sure to move around the gas dispension tube when gassing the solvent so as to avoid clogging the tube.


killerbeezzz

  • Guest
A/B
« Reply #2 on: October 21, 2004, 12:21:00 AM »
He did a standard A/B extraction and got about 30ml of very light brown oil.  The oil is said to taste exactly like the other MDMA that he has tasted.  He is thinking that he will distill the oil but is not too sure because he fears that he will loose too much to the glassware.  Is it alright to just put the Freebase in the NP and gass?  Last time he gassed with out the A/B and got crappola

jackhole

  • Guest
Distill if you care about your health
« Reply #3 on: October 21, 2004, 03:45:00 AM »
You don't have to distill and your customers won't care, but over the long-term, serious side effects can induce from undistilled MDMA base contaminated with intermediates. These intermediates can alkylate your DNA and thus increase your risk for cancer. So, if you care for your health, you'll distill and sacrifice some yield. On the other hand, if your eye is on the dollar, just crystallize your product.

Btw, recrystallization cannot remove the impurities that a distillation can. For a pure product, you MUST start off with clean precursors, perform the A/B correctly, distill, and follow that by a few recrystallizations. Hope this helps.


indole_amine

  • Guest
steam distillation
« Reply #4 on: October 21, 2004, 05:04:00 AM »
If your amount of freebase is so small that regular vacuum distillation would cause too much losses, you can always try to get hold of some micro-distillation apparatus (suitable for volumes of 1-10ml  ;) ) or some micro-scale distillation rig - or even better use steam distillation (distill at atmospherical pressure, together with water). Although it may take some time (MDMA freebase isn't very volatile with steam), the purity is as good as with vacuum distillation, and the losses are minimized. Downside is the long time it needs and the extra a/b, drying and solvent removal you'll have to perform afterwards - but it is worth the work.

Together with max. 3 recrystallizations (nice dual-solvent/cooling procedure, not evaporating everything or flooding with acetone!), you'll get an outstanding purity, and gassing becomes alot easier, too!

(promised!  ;) )


indole_amine

DoctorFeelgood

  • Guest
freebase distillation
« Reply #5 on: October 21, 2004, 05:55:00 AM »
i distilled the same amount like you a couple of times. therefore i used 2 small distilling flasks (e.g. 100ml) and a 250mm distilling bridge (about 60 dollar/euro all together). with wateraspirator vacuum the bp is about 150-155 C - in my case. don't be in a hurry, loss is about 5 percent (max. 10%) - mostly redish trash in your distilling flask. the freebase is waterwhite. dissolve it in NP, after gassing you get a snowwhite powder. then recrystallize this snowwhite powder e.g. in hot IPA, you will get big rockhard crystals.
believe me, you can even feel the difference, it's much stronger, sure the purest stuff in town...

"The oil is said to taste exactly like the other MDMA that he has tasted"

i know this problem. the so called 'typical' mdma taste/smell is just a sign for impurities, in my case it smells like nothing and it tastes bitter. if one offers you a brown 'pure' powder - forget it.

indole_amine

  • Guest
losses = impurities?
« Reply #6 on: October 21, 2004, 06:01:00 AM »
And I bet that most of your "losses" are indeed the impurities which stay behind as brown goo...

I wouldn't say that MDMA freebase is odorless - it is just a very faint odor, compared to MDP2P or safrole. Take a small drop and rub it between your fingertips. It WILL smell... (make sure to wash your fingertips in orange juice and drink that afterwards!  :) )


indole_amine

killerbeezzz

  • Guest
A Distilling he will go
« Reply #7 on: October 21, 2004, 08:46:00 AM »
Swim is convinced about the distilling of the FB.  He has a 50ml and 100ml flask.  Since he is making this for personal and friends use there health is important.  Say he gets about 27ml of freebase after distilation about how much salt should he have after gassing?  And is a slow or fast gassing the way to go?

runne

  • Guest
The need to gas instead of titrate AFTER distill?
« Reply #8 on: October 21, 2004, 10:40:00 AM »
If you did a proper A/B, and a proper distillation of the MDMA freebase, would there be any major problem with just titrating the oil and evaping? Same purity?


jackhole

  • Guest
27ml FB -> 30g HCl
« Reply #9 on: October 21, 2004, 11:55:00 AM »
27ml of freebase will afford you with around 30 grams of the hydrochloride salt. You can calculate the exact amount by calculating the percentage that 27ml MDMA base is to 1 mole of MDMA base, and multiplying that factor by the molar weight of MDMA hydrochloride.


indole_amine

  • Guest
precipitation methods other than titration..
« Reply #10 on: October 21, 2004, 02:49:00 PM »
evaporating will always result in slightly acidic amine salt; you'll have to wash it thoroughly with acetone to remove this HCl residues. Or you titrate to perfectly neutral pH 7: then you'll have to repeat titration very often until you get all your fb. The advantage of gassing vs. titrating is that the solvent holds back more impurities, contrary to the aequous amine salt solution after titration - it carries some of them over to the final dried product.

If you want to avoid gassing, you could always neutralize your amine free base by dissolving in nonpolar and adding an equimolar amount of anhydrous HCl/IPA (works really good), or you could use one of Bandil's ingenious new crystallization techniques with either azeotropic drying or molecular sieves (they both use aequous HCl without gassing!).  ;)


indole_amine

killerbeezzz

  • Guest
Drying
« Reply #11 on: October 21, 2004, 06:09:00 PM »
So if Swim is going to gas with distilled FB and new Xyelene would he need to use epsom salts to dry the solution?  Also what is the best way to generate HCl.  He has used the muric acid dripped into sulfuric acid with a drying column method.  He is thinking that the Sulfuric dripped onto NaCl and muric with the drying column is the way to go.  Does anyone have experience with both? 

The gassing set up that he is thinking about would go like this.  A 1000ml two necked round bottom flask with a 125ml dropping funnel in one neck and a 200mm packing column in the vertical neck.  The packing column would be loaded with DriRite  and at the top would be a thermometer adapter with some aquarium tubing stuck in it.  From there it would go into the gassing chamber that is a jelly jar with 2 holes in the top.  One hole has a rigid tube that  goes to the bottom of the jar and the gas will come in there.  Then he will have a hole with a tube just inside of the jar that is the outlet.  That would go in to a 2ltr soda bottle with a saturated sodium bicarb solution to neutralize the Hcl gas.

indole_amine

  • Guest
yes - drying is necessary
« Reply #12 on: October 21, 2004, 09:30:00 PM »
You should dry your xylene before dissolving your freebase in it. Or you might end up with lots of dissolved MDMA*HCl... :(

For anhydrous HCl gas, just drip 99% sulfuric onto NaCl, and use a drying tube. Best would be to fill it with some silica gel, predried in the oven at 220°C - Drierite or CaCl2 is not very good in fast gas drying. And better give your sodium bicarb bottle an outlet hose, too - not all HCl will be absorbed, and you schould vent these HCl fumes to the outside (with a long hose) if you like your lung tissue...

Everything else sounds very nice. Good luck, and report back!  :)


indole_amine