Author Topic: Alternative To Gassing Ideas?  (Read 10457 times)

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Barium

  • Guest
True, very true! There are other acids to use ...
« Reply #20 on: October 08, 2002, 10:00:00 AM »
True, very true! There are other acids to use besides HCl. Try citric-, acetic-, tartaric-, phosphoric- and sulphuric acid, to name a few.

Catalytic hydrogenation freak

ballzofsteel

  • Guest
old news
« Reply #21 on: October 08, 2002, 12:13:00 PM »
Hows about sticking your mix in a soda pop carbonation device,such as a soda stream.Cheap,clean,efficient.
Seems like it was designed for this purpose. ;)

Does carbonate form with MDMA?

Rhodium

  • Guest
Yes, MDMA carbonate can form.
« Reply #22 on: October 08, 2002, 12:24:00 PM »
Yes, MDMA carbonate can form. Carbonates are pretty unstable salts though.

moo

  • Guest
carbonates
« Reply #23 on: October 08, 2002, 01:11:00 PM »
But the soda pop carbonation device won't produce carbonic acid on its own, the carbon dioxide has to react with water first. Theoretically there has to be one mole of water per two moles of an amine freebase. (CO2 + H2O --> H2CO3)

yellium

  • Guest
To the original poster: ever tried to UTFSE?
« Reply #24 on: October 08, 2002, 02:22:00 PM »
To the original poster: ever tried to UTFSE?

When all you've got is a nailgun, every problem looks like a messiah...

Rhodium

  • Guest
meth carbonate smoking
« Reply #25 on: October 08, 2002, 02:42:00 PM »
Madmax: Yes, as methamphetamine carbonate decomposes to the freebase upon heating, smoking it is essentially like smoking the freebase, i.e. stronger, faster, etc., yet it is still a convenient to handle solid.

carboxyl

  • Guest
With MDA, you could obtain the ascobate using ...
« Reply #26 on: October 08, 2002, 03:57:00 PM »
With MDA, you could obtain the ascobate using Vitamin C which is supposed to absorbed by the body quicker, and be more potent (see

Post 59321

(LaBTop: "Re: MDMA chirality", Serious Chemistry)
).

The above post is purely fictional. Any resemblance to "real-life" is purely coincidental.

starlight

  • Guest
with regard to storing pre-gassed ether
« Reply #27 on: October 09, 2002, 02:13:00 AM »
if you distill ether from starting fluid, it is not a good idea to store it too long. When distilled, the ethers (normally a mixture of diethyl/di-isopropyl) will have no stabilizers, and will be prone to the formation of explosive peroxides. It is suggested above to store it in the freezer. This may or may not help, I have no idea and would not like to find out myself.

Also be aware that storing extremely volatile solvents in non-lab freezers can create powerful explosions if the solvent vessel is not absolutely air-tight. Otherwise solvent can escape and be sparked off by the thermostat.

Bwiti

  • Guest
acetate
« Reply #28 on: October 09, 2002, 04:30:00 AM »
In my dreams, I've had the acetate and hydrochloride of MDMA; both kick in at approximately the same time. One could always dissolve the freebase in a tiny bit of glacial acetic acid, then put a fan on it to dry, but you might want to make plans to leave it behind a closed door for 2 days unless you don't value your mucus membranes, lungs, and eyes. If the freebase was dissolved in toluene or ether, then acetic acid slowly dripped in, would the goods precipitate out?

Love my country, fear my government.

hermanroempp

  • Guest
Alternative to gassing?
« Reply #29 on: October 09, 2002, 01:20:00 PM »
Maybe...
One (very old) method is to simply shake ether (ether must be used) with concentrated hydrochloric acid in a sep funnel. Most of the HCl will dissolve in the ether by forming the oxonium compound, creating considerable heat, so expect to vent your sep funnel very often! The water phase (lower phase) is now drawn off and discarded and the ethereal HCl solution (upper phase) is saved. All you have to do now is to titrate a ethereal solution of your amine with the ethereal HCl solution to get the hydrochloride.
As I know from personal experience this methods works best with
a) amine hydrochlorides which are not too hygroscopic and
b) lots of ether used for the amine solution
because the HCl/ether solution contains still some water, which will stay dissolved if lots of ether are used.
This procedure works for sure with some alcaloids (atropine, quinine), so you could give it a try on a small scale for your preferred "alcaloid".  ;)

Quidquid agis, prudenter agas et respice finem!

Rhodium

  • Guest
I think that ether usually dissolves 7-8% water.
« Reply #30 on: October 09, 2002, 01:38:00 PM »
I think that ether usually dissolves 7-8% water.

Alcohol, an unconsciousness-expanding drug

TheBlindGenius

  • Guest
Using anhydrous Calcium Chloride??
« Reply #31 on: October 09, 2002, 06:02:00 PM »
So if CaO + HCl __> CaCl2 + H2O, then what happens when you add a buttload of anhydrous CaCl2 to a solution of alcohol or ether and 37% aq. HCl?  Does it remove the water?

Rhodium

  • Guest
Yes, it will absorb water, but as HCl also is ...
« Reply #32 on: October 09, 2002, 06:14:00 PM »
Yes, it will absorb water, but as HCl also is hygroscopic, I don't know which compound would pull hardest and keep the water. CaCl2 will catalyze the chlorination of alcohol to the alkyl halide though, causing a mess.

Alcohol, an unconsciousness-expanding drug

Diggity

  • Guest
GASSING TIP!!
« Reply #33 on: October 10, 2002, 12:55:00 AM »
IF YOU ARE HAVING PROBLEMS GASSING.. LET ME HELP!!

After fuckin around, I found this to be factual, and interesting.

Swim has a bubbler setup, and noticed something interesting a few weeks back.

He had 2 containers in which he was preparing to gas 1600ml's of nonpolar/freebase

One of the containers was a large 2L pyrex measuring cup, and the other, a 1L beaker.

Each were filled with 800ml's of the nonpolar/freebase.

Using the exact same bubbler setup on both gassing runs, the 1L beaker filled with crystals wayyyy faster then the 2L meauring cup.

This leads me to believe that the taller and slimmer the vessel is, and the lower that gas distribution tube is, in the non polar, the faster your shit will get done.

I think it has to do with the hcl gas bubbles traveling upwards through the non polar crashing out more crystals than if the tube was 10mm into the solution, sitting in a lowform dish, like the 2L pyrex measuring cup.

This may help some, this may go unheard, you may not give a flying fuck, either way, it works for sure. Swim tries his hardest to make sure no variables are changed when he experiments. The 1600ml's were from one batch, just split in 2.

Each produced about same amount. One was just done faster. I bee on the hunt for a super thin, very long/tall vessel to use.. experiment further..   :)

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

endo1

  • Guest
I only have access to smaller chemical companies ...
« Reply #34 on: October 10, 2002, 01:08:00 AM »

I only have access to smaller chemical companies that do not carry HCl/IPA or HCl/MeOH


When SW is gassing 2000 ml IPA w HCl w stirring, he can gas it quite a bit before there's any residual fumes at all. It does fume a little bit when the solution is poured but it's a much nicer system than gassing product disolved in toluene or ether fume wise.

Diggity

  • Guest
If you do shit right, and got a lab separate from ...
« Reply #35 on: October 10, 2002, 01:16:00 AM »
If you do shit right, and got a lab separate from your home, and it's out in the middle of god know's where! LIKE IT SHOULD BE, then it's all good, in fact! It's all right!! You know the rest..  fuck all day.. fuck all night, and gas in gas in peace. Just set up a table by a window with the fan blowing out and you can fall asleep next to it and not smell a damn thing.

Swim has never gassed anything but toulene, so he wouldn't know the joys of gassing ipa..  :(  

He would like to titrate into dcm someday. He really enjoys smelling dcm. It's so bubblegumish. Makes him happy when he smells it.  

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

Rhodium

  • Guest
HCl gas corrodes everything in a matter of ...
« Reply #36 on: October 10, 2002, 02:26:00 AM »
HCl gas corrodes everything in a matter of minutes - I hate working with it. It even discolors stainless.

HCl in DCM? I wouldn't reccommend it for amine crystallization, as many salts (like MDMA.HCl) are partly soluble in DCM.

Alcohol, an unconsciousness-expanding drug

Bubbleplate

  • Guest
Until SWIM Decided Gassing was just more trouble
« Reply #37 on: October 10, 2002, 03:54:00 PM »
than it was worth, she had planned on using one of those "Pyrex  Gas Washing Bottles". You know, the kind that has a removable top and is taller than wider. Plus it has an Inlet to gas the product, and an Outlet that could be run to a basic solution or vented.
Oh yeah: someone posted that they had inhaled HCl gas. ALWAYS keep a bottle and rag of Ammonia (dilute!) around. If you accidently inhale, it could save your lungs. Breathe a little in.
I've seen plastic Keck clips around GG joints crumble to dust from HCl gas...

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

Diggity

  • Guest
Wow, you guys have serious issues with HCL gas..
« Reply #38 on: October 10, 2002, 04:32:00 PM »
Wow, you guys have serious issues with HCL gas.. it doesn't bother me any. I always set up shop next to a window with a fan blowing out it and nothing ever gets fucked up, especially my lungs.. I can't even tell im gassing anything, except fot the sound of the bubbles.

My only complaint is the length of time it takes to reach completion.

1600 ml's of freebase containing 50g of product takes a good hour to finish..

Ive heard bee's say they gassed half that amount in 5-10 minutes..

Maybe it's the power the dual headed fish tank pump is providing. Not enough? Not bubbling hard/fast enough? Will get another pump, and add 2 to the mix, maybe that will cut the time in half.. 

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

Chicken

  • Guest
HCl gassing
« Reply #39 on: October 10, 2002, 04:45:00 PM »
Swich just sets up the flask that the prodcut is being gassed in with a two hole stopper, and insterst glass rods trough both holes, and then attaches tubing to the two tubes. One of the tubes is a J tube that runs into  the product (or a gas dispersion tube) and then other only goes partially into the flask. A tube is run from the outlet tube to the outside through a window, hence all the hcl gas goes outside. Whats so hard about that? Just bee careful on a still cold night in an urban area.  Swich has a bad memory of a doing this in a downtown apartment in a metropolotin area, and seeing an entire city block covered in HCl fog from only 30 minutes of gassing.  Let me tell you Swich was suprised as hell when they walked out the back door of the apartment and saw and urban street covered in a fog on a 10C (50F) night.  Swich has since learned not to do such things in apartments, but if you are an apartent bee, and trying to gas, using this tube venting method be forewarned . . . it's probably the same with a fan, but Swich has never used a fan, always done it this way, until Swich had a fume hood, and then the tube was routed into the fume hood, and it carried away all the hcl gas.  Either of these methods wil make almost 0% hc gas onto the reaction area, with no smell.  Bt then again every now an again a stopper will blow out, if you don't seucre it properly.  Thats when it;s nice to be using the dripping hcl into H2SO4 method of Hcl production.  You can just turn it off.  If anyone is in the lab with you when the stopper blows off when you are gassing I gaurantee they will FREAK out -- hehe at least thats my experience.