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Alternative To Gassing Ideas?

Started by Bubbleplate, October 07, 2002, 06:23:00 PM

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Osmium

> Maybe it's the power the dual headed fish tank pump is providing.

Maybe a fish pump bubbling air through HCl isn't the best and fastest way to do this?

I'm not fat just horizontally disproportionate.

Diggity

Maybe Os is right..

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

Osmium

Never know until you try...

I'm not fat just horizontally disproportionate.

Diggity

Try what!?

I was thinkin.. I have this Gast piece of shit I use for vac filterations.. it has an dual head, intake and exaust.. I could hook it up to the exaust and get 100x the power, but that may be toooo fast.

I guess I'll never know till I try..

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

Bubbleplate

SWIM was visiting a friends lab during gassing and they had dripped way too much H2SO4 into the HCl & NaCl. Next thing, foam galore and suddenly not only is a Stopper blowing out, but a stream of HCl and conc. H2SO4! Luckily SWIM had a full face shield, hat, and Kevlar jump suit and not just goggles and dungarees!
Newbees, are you taking notes?? Bee safe! Your eyes and face are worth $100 of protective gear.

Diggity

H2SO4 dripped onto NaCl

Wouldn't that produce mdma sulfate though?

As soon as he gets a rotovap he will distill his freebase and gas a smaller volume of non polar, rather than gassing such a large amount.. I don't know if that will speed up the process, but it cant hurt..

Would adding some NaCl to the bubbler containg the hcl produce more hcl gas, than without??? Swim has yet to try that..  

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

SPISSHAK

Stick a plastic tube up yer butt and bubble away.
You might want to use a trap or check valve, beecause toulene up yer ass is no fun, trust me.
This is what's been done,all jokes aside, titurate the freebase solution (with hydrochloric acid)and azetropically distill off the water as a toulene azetrope, watch crystals appear. works just almost as well as gassing, but SWIS likes to gas , SWIS uses a coke bottle, drill two holes in the cap, fill with salt and HCl wrap teflon tape around the threads, place cap, use rubber as a 'gasket' for your tubing, fill a basting syringe with sulfuric acid, and drip onto the Hcl salt paste, gas away.
This thread should be in the newbee forum.

goiterjoe

Wouldn't that produce mdma sulfate though?

No, and you seriously need to learn a lot more before you hurt yourself.

All paths are the same: they lead nowhere

ClearLight


  so is the idea with the hcl in the IPA, that you heat the ipa to liberate the hcl, or do you drip the IPA into the freebase/solvent mix?



Infinite Radiant Light - THKRA

hCiLdOdUeDn

Diggity,

H2SO4 + NaCl ---> Na2SO4 +HCl

The HCl used to gas the mdma freebase to mdma.hcl

To bee or not to bee, that IS the question.

El_Zorro

hidden cloud:

according to argox, it's NaCl+H2SO4 --> NaHSO4+HCl.

No shit, this should really be in the newbee forum.  However, I would like to know bees' opinions of the shelf life of various stock solutions of NP solvents and HCl.  Namely, IPA, MeOH, Et2O, acetone, etc.  They can't sit around forever, the HCl would react.

Who is that masked man?

TheBlindGenius

OK, swim has decided to try Argox's method as outlined on Rhodium's page.  He has some questions though.  First, can the trap be eliminated if one just uses an inverted funnel in the receiving flask?  That's what we do in analytical chemistry to prevent suckback when distilling ammonia into HCl, would it work in this case?  It would make the apparatus much simpler.  Also swim doesn't have any of those fancy "custom 3-way adapters."  Could he just use pinch clamps on the hose?  Another thing.  Swim just wants a mole of HCl (36.46 g), which should be enough to react w/ 192.7 g MDMA freebase or 178.7 g MDA freebase.  What would be a good amount of IPA to dissolve one mole of HCl at room temp?  Rhod said they sell 5 M right?  so 200 mL should be fine?  Anyways, how would I standardize my solution when I was done?  Just like if it was aqueous HCl?  Or differently?  One more thing, does a 5 M solution of HCl/IPA fume at all?  And is it stable at room temp or should it be stored at a low temperature?

Rhodium

If you put pinch-clamps on your HCl gas tubing, make sure that any over-pressure inside the apparatus doesn't blow a stopper out (or worse). Use at least 250ml IPA to dissolve one mole of HCl, and chill the IPA with ice when gassing it - the solubility goes down fast above room temp. Standardization of the solution is probably best performed by diluting a sample to 50% with water, add some bromthymol blue indicator and titrate with 0.10 M sodium hydroxide until the color changes. 5M HCl in IPA fumes violently, at least as much as conc aqueous HCl. Room temp is okay, but the cooler the better. Never fill your storage flask more than 2/3 full, and expect overpressure every time you open it.

Rhodium

Chill your alcohol solution thoroughly, or else some of it will evaporate during the exothermic dissolution of the HCl, making you miscalculate the concentration afterwards.

lab_bitch

To get the maximum amount of HCl gas absorbed in the freebase/alcohol/ether, you want to use a tall, slender vessel with strong agitation.  The taller the vessel is, the more contact time each bubble of HCl has with the solvent, so more mass transfer can occur.  Agitation breaks the bubbles into smaller bubbles, disperses them throughout the vessel, and increases the concentration gradient around each bubble.  All of these increase the rate of HCl absorption.  Fast stirring is absolutely essential to getting higher yields based on the amount of HCl gas used.

ClearLight

so could an ultrasonic agitator be used?


Infinite Radiant Light - THKRA

moo

Ultrasonics are used to degas solvents. You would end up with what you started with.

TheBlindGenius

Anyone have an opinion on getting rid of the trap and using an inverted funnel?  Also, how can I analyze the water content of the final solution?  Is there any special instrument that is used for this?

El_Zorro

I guess if you just wanted to know if there was any water present at all, you could just take a sample of the solution in a test tube and add some anhydrous cobalt chloride, which will turn fro blue to pink in the prescence of water.  If you're looking for the amount of water in solution, I have no idesa what you could do.

Who is that masked man?

SPISSHAK

If water is present it will appear turbid, and in some solvents you can correct this by adding something that will azetrope with water, and then distill the azetrope off through a dean-stark (or whatever).
You would want to use this azetrope method if you goofed during an extraction, and did'nt want to use drying agents for fear of precipitating your good-stuff onto the drying agent as it absorbs water.