Endpoint titration of MDMA

[nitrous351]

This question was asked a couple of months ago, but nobody ever gave a straight answer. I put "MDMA titration" in TFSE and came up with 18 threads, and none of them helped me. I don't want to pay $100 to send my pressed pills off to a lab to get quantitative results. I don't want to anonymously send a pill to dancesafe to get results. I don't want to make up a Marquis reagent to test for the presence of a MDMA-like substance. I want to titrate to an endpoint on my own so I can quantitatively analyze a pill's MDMA content. So, with all that out of the way, anybee have suggestions on which indicator/titrant i should use? Thanks!

[Barium]

Covert the amine hydrochloride to the freebase and extract it, then crystallise it again. This is the easiest way to get a rough figure of the amine content. But remember that you can't distinguish MDMA from MDA, MDE or other amphetamines this way. To do that you have to separate them using chromatography.

[raffike]

not only primary and secondary amines come
dimethylated stuff will also come over and all other nitrogen containing impurities.

[Barium]

Therefore the need to separate them by chromatography

[bones]

im not sure that titration would work... given that if you titrate the acid into the freebase.. you would form the salt.... and viceversa.... honestly ive never used titration to determine concentration of such a compound... and im not sure that it is possible... however given that im wrong remember the tiny volumes we're talking about...practically it would be too hard and not accurate.... not in my opinion anyway... but then im not a very good chemist ...

seperation of the pills contents via anything but hplc would also not be practical for determining pill quality for the following reason.

matter cannot be created or destroyed... except in fission reactions and column chomatography.  in my experience no matter how much solvent you put on you never get back everything from silica colums...  but again.. im not the worlds greatest chemist ..

again i dont believe this method is practical for determining accurately determining mass of mdma... nice for prification though if you can be bothered... and have the gear...

my best advice is to examine it via TLC... that will give you an idea of the number of compounds present.. im sure you can find rf values for given compounds with given solvents with given plates... wont give you masses.. but its a suprisingly sensitive technique ..

[Aurelius]

if you want more efficient methods of separation, try HPLC.  (yes, i know not everybody has access to the equipment for this- at least not a ghetto-rigged setup)

[raffike]

If MDMA would be freebased,it could be analysed with GC also right?Lil offtopic but...at least in former soviet union they used hydrogen gas in GC as a carrier,when gas came out of other end of column,it was set on fire and flame temp was recorded to get some sort of graphic.Do they use this method anymore or is only MS used now?

[Rhodium]

That method is still used, but it isn't as crude as you make it sound like. It's called a "FID" -

Flame Ionization Detector

(http://www.uga.edu/srel/AACES/GCtutorial/page17.html)

[raffike]

hmm...Rh,i think you meant something else,these soviet ones used some kind of sensor to just monitor the temperature.When hydrogen gas is mixed with some organic substance,the temperature of the flame is different.When H2 gas couldn't be used as carrier,like it was too reactive or something,then pure H2 was mixed with carrier gas after it had passed the column and then flame temp measured.Column temp was usually kept around 180C.It sounds pretty robust to me but apparently these GC's worked.