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HCL gas

luminouspath

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29 Mai 2013
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What are peoples recommended methods for producing HCL gas? I've read this - https://www.erowid.org/archive/rhodium/chemistry/hclgas.argox.html and produced it successfully with H2SO4 and HCL, but I don't have enough glassware to make the IPA bubbler stage the author describes. The method using H2SO4 and salt seems like it wouldn't produce enough HCL gas and could lead to very tedious clean-up.

If I leave out the IPA bubbler will the HCL gas produced be anhydrous enough not to fuck up my product? Or is it necessary?

Thanks
 

Moriarty

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28 Avr 2007
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Actually, the easiest way in my opinion to make HCl(g) is to add 31% HCl(aq) to CaCl2. HCl gas will start to evolve immediately. Calcium chloride is a very effective drying agent and it absorbs thewater that the HCl(g) is dissolved in causing the gas to be released. This is a little exothermic so some water will get carried away with the HCl but this is just lead through a short drying tube and then into the MDxx/non-polar solution.

Moriarty
 

piuiher

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19 Nov 2012
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Dripping H2SO4 onto NaCl works well and evolves little to no heat. It s slower though and probably not advisable for big quantities.
 

Moriarty

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Well, keep in mind that both have their advantages and disadvantages. It sort of dawned on me when piuiher mentioned the speed of HCl production via H2SO4/NaCl. The speed at which HCl is produce by the reaction between H2SO4 and NaCl is slower but really manageable. The first time I ever did this I wasn't really sure how exactly to proceed so I made my system in a fashion that made sense to me. So I put together the whole distillation set-up. This was a long time ago but let me see if memory serves. This meant I put the whole thing together. So first a lab stand was brought in and then a 500ml round bottom flask which was about half full with NaCl was clamped to the stand. On top of the 500ml boiling flask was fitted with a claisen adapter. On top of the Claisen adapter is obviously the need to fit two pieces. On the side arm of the adapter was placed a dropping funnel with H2SO4. The top of the adapter was fitted with a distillation head (75 degree adapter) and a stopper/plug on top of that. Now I was ready for the west condenser. First, notice that pretty much every West condenser in the world has these three glass prongs in it so that the condenser can be used for more than just a condenser. In this instance I added a small piece of cotton but, in retrospect, just a small piece of tissue paper would have worked just as well. Now the condenser was filled about 80% of the way with CaCl2 and this made for a decent drying tube. Now the vacuum adapter was fitted and clamped. I used a piece of surgical tubing and placed that, somehow, on the end of the vacuum adapter. Okay, so now this whole giant set-up with way, WAY too many pieces was brought to a level where the tubing was about over the xylene/MDMA solution. Now all that remained was to let in H2SO4 as needed to produce HCl gas and lead it out to the beaker holding the goods. There were several problems with this set-up/ One it had too many parts. If I had done it this way more than a few times I would have surely started breaking pieces. Second, surgical tubing is a little soluble in xylene, so towards the end of the gassing my tube was dissolving at an alarming rate into the mess of MDMA/MDMA.HCl/xylene/latex surgical tubing. Go-go gadget acetone ;-)! The advantage was that I could easily control the amount of HCl being produced in the system by just adding H2SO4 slowly. Overall, if I hadn't abandon H2SO4/NaCl, I would have had to streamline that whole set-up but the advantage of producing gas according to my needs was a plus.

When you produce it with CaCl2 and HCl(aq) the whole thing gets simpler...or it gets simpler than my overly complex monstrosity of a system. Instead of a boiling flask ye ol' 1.5 liter water bottle is used. Now, keep in mind that when you add HCl(aq) to CaCl2 you get lots and LOTS of HCl very quickly. Also, even though the HCl(g) starts to get produced more slowly with time, if you need to slow it down considerably to say filter out some of the MDxx.HCl, there is no way. The only way to stop the production of HCl gas in this set-up is to quench the whole thing with water and start over. Anyway, all one need do with this is fill a 1.5 liter water bottle 1/2 to 2/3rds full with CaCl2. I used to use lots of 19/22 glassware, so this sort of utilizes that. On top of the bottle was placed a 24/40 to 19/22 bushing adapter and this was taped together with electrical tape. Now I placed a 19/22 distillation head (75 degree adapter) on top of that. A plug was added to the top of the distillation head and electrical tape was used to keep that in place as well as seal leaks. Now a West condenser was fitted with some tissue paper (just enough to keep the CaCl2 from falling through end of the West condenser) and the condenser is filled with CaCl2. This was taped, again with electrical tape, tightly to keep the condenser in place as well as to keep HCl(g) on the right path by stopping leaks. To the end of the condenser was added a piece of polyethylene tubing and that was taped in place very securely. Notice the only part of this whole set-up that I not taped together well is the place between the bushing adapter and the distillation head. This is so that you can add 31% HCl(aq) as you desire. This system works well enough. Just make sure that the amount of HCl(aq) you add is small in the beginning. The speed at which HCl(g) will evolve will depend upon how much HCl(aq) you add and the size of CaCl2 you are using. In the U.S. the CaCl2 that is available without going to a lab supply company is medium sized chucks. Traditionally adding 50ml of 31% was not too much for the CaCl2 that was being used but if you had finely powdered CaCl2 it'd all happen way too fast and much less HCl(aq) would need to be added. Just go slowly until you figure it out...like add small amounts at first...10ml or so. Otherwise you won't be able to keep the thing together and the last thing you want is to make a HCl(g) bomb!!! Also, you must blow a small amount of air through the whole apparatus first to make sure gasses may flow through this thing before you start adding HCl(aq). Otherwise, again, you won't be able to keep this thing together.

Moriarty
 

luminouspath

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29 Mai 2013
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Is the CaCl2 drying tube/condensor necessary with the H2SO4/NaCl method? I've read somewhere that it should produce dry HCL(g) and sodium bisulfate. The CaCl2 + HCL method sounds very workable, will probably go with that.
 

Moriarty

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28 Avr 2007
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Well, when produced from NaCl and H2SO4 there won't be any water produced but, assuming the H2SO4 you have isn't 100%, there is probably some water present. It stays pretty dry. Really, a drying tube is good form but it won't hurt anything if you don't employ one.

With CaCl2 and HCl(aq) more water is present. A drying tube is a good idea with both but more necessary here.

Moriarty

P.S. The reaction between H2SO4 and NaCl produces HCl and Na2SO4 (sodium sulfate).
 

im1badpup

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10 Sept 2008
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290
I dripped hcl onto always an excess of h2so4 (stirred). The hcl gas worked very well without needing any further drying. If the solvent was completely anhydrous 'snowflake' in appearance crystals would initially form floating around until enveloped in the wallpaper paste crystal mush as they ran out of room.
 

Moriarty

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28 Avr 2007
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That gas is horrible, is it not. I love that fluffy white precipitation. It's easier to wash the impurities out of with acetone than other methods on forming the HCl salt but isn't it nasty ;-)? In any event, it had never occurred to me to form HCl(g) in this fashion. Cleaver.

Moriarty
 

im1badpup

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10 Sept 2008
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I was originally at the time going to follow what youve described moriarty as the safest practical method.. got caught short missing the 'tape' at stupid o clock and went for another method on a ghetto rig instead... doesn't take much of a leak to be coughing and a snotty nose that's for sure lol. Aquarium air pump tubing [the clear stuff] works great in the solvent without any detioration over a night n days gassing though. soft enough to squeeze any product out stuck up there when finished too if a bit sucks back up.
 

im1badpup

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10 Sept 2008
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290
I was originally at the time going to follow what youve described moriarty as the safest practical method.. got caught short missing the 'tape' at stupid o clock and went for another method on a ghetto rig instead... doesn't take much of a leak to be coughing and a snotty nose that's for sure lol. Aquarium air pump tubing [the clear stuff] works great in the solvent without any detioration over a night n days gassing i can attest to that. it may be better than the surgical stuff, ive never used it tbh . soft enough to squeeze any product out stuck up there when finished too if a bit sucks back up. 'madprosser' originally suggested the hcl onto h2so4 in a thread on here similar to this one back in 2009... i was probably the thread starter then with a question almost identical to luminouspaths funnily enough. i think he [madprosser] referenced argox as to the proper setup to use. was a busy site back then, its quiet as now.. Apoligies im having trouble staying logged in so posted then edited and then double posted by mistake. the 'new' site layout is alien to me il find the delete unwanted post button soon.
 

im1badpup

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10 Sept 2008
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Well id just figure an healthy excess, completely unscientific like. Eg 150ml 95 percent sulphuric for 20ml 28percent hydrochloric.
 

rosa

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15 Nov 2013
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HCl salts are best achieved as Moriarty first said, calcium chloride and muriatic. I strongly encourage HBr salts (NaBr +H2SO4 and treat as muriatic as above) for increased bioavailability of MDX as well as an easier time on blood ph (Adding hcl ions to the stomach disrupts blood alkalinity). Muriatic is not above gakking and iron excess and nabr/sulfuric are pretty pure domestically right now otc ime.
 

Moriarty

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28 Avr 2007
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I have a question concerning bioavailability. My father, a pharmacist, told me as a child that different salts had different absorption times and, presumably, bioavailability. Then a guy at the Lycaeum, who claimed to teach pharmacology at a University, said the salt formed didn't matter and had no affect upon absorption time or bioavailability. I truly do not know the answer to whether or not different salts work differently in the body.
 
C

CheesePizza

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Depends on the liposolubility of the salt (example : succinate VS hydrochloride).
 

Moriarty

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Thank you very much! I have always wondered about this. It is good to have a conclusive answer. I guess I should have listen to my father. After all, he is a practicing pharmacist!!!

Moriarty
 

rosa

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15 Nov 2013
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The PH of the stomach cannot be ignored in this discussion.

So, let's talk about that first, sorry for the tangent.

Most amphetamines are better absorbed after antacids are taken. This is true for amphetamine, and more true for MDMA. The methylenedioxyring is easily digested by the stomach if the stomach is filled with excessive acid, in addition to the absorption being slowed, which is a double fuck you.

Spisshak (however he spelled it) talked about MDMA citrate a bit. Around that time in a certain lab MDA was more disposable, so MDA HCl and citrate were both made and tasted. The citrate was not well liked. It felt like a bunk bean, a fuzzy experience that was ill defined. But it certainly lasted longer.

The acetate took up moisture and was fuzzy, the tartrate and fumurate were no better. All of the weak acid salts were meh. The jewel of the series was the HBr, it came on fast and hard, and was as potent and long lasting as the weak acids, and was analogous in its manufacture (once aqueous hydrobromic was obtained from bromide salts and sulfuric which is as easy as can be and clean) to the hydrochloride, and just as pharmacologically acceptable of a salt, free flowing, stable, and of a generally preferable crystal structure.
 
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