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  • AADD Moderators: swilow | Vagabond696

Latest DEA Microgram report

mind said:
phase_dancer:
most labs in the Netherlands work with the leuckart method.
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From my knowledge, the most common methods are either hydrogenation using methylamine gas & catalyst (large scale) or the 'cold method' using NaBH4 with CH3NH2 in methanol. The cold method can be carried out in any handly vessel & can be done by a trained chimp. I've seen a lot of stuff made in The Netherlands and I've never seen the leuckard method used. Why would you? It's messy, smelly and uses a chemical even MORE watched than methyl amine (the PMK is a given).
Oh, and hobbiests use the Mercury amalgam method since it's handy for kitchen sink scale.
 
haribo1, I agree with your reasoning regarding the Leuckard route. I could never understand why anyone would prefer this method unless of course the chems were the only ones available.

As for Australia; formamide, N-methylformamide and sodium borohydride are watched chems in Australia. All are available to supply company account holders without problem, but the general public has to complete and end user declaration (EUD) form, making them out of reach for many would be producers. Hydrongenators also tend to arouse suspicion as do hydrogen gas cylinders and raney nickel which are restricted items.

However the cold method or "cold fusion" method as it's termed here, is occasionaly mentioned in news stories on lab busts.
 
afaik the reductive amination doesn't use very high temps, although some methods report that heating the mixture increases speed of reaction. From memory, other methods actually cool the mixture. I looked into the various techniques some time ago while doing a Uni project on MDP2P impurities.

Please do the ICP but only if you can do so without getting into trouble. Reports on a few tested samples would be fantastic but I'm probably pushing my luck here ;)

Do you use ICP-OES or MS?
 
Hey, whats MDDMA like?, (december report).

ECSTASY COMBINATION TABLETS (CONTAINING MDMA,
METHAMPHETAMINE, AND MDDMA) IN MIAMI, FLORIDA
 
Its an impurity found in a certain synthesis of MDMA.
 
MDDMA or MDDM as Shulgin calls it is produced during reductive amination using dimethylamine. This is a commonly reported impurity in some commercially sourced methylamine (& homemade). You'll note only a trace was reported, backing this theory. However, unless you like taking large amounts of a substance that may give you an unpleasant experience and leave you without a sex drive, I'd give MDDMA a wide berth.

From PiHKAL#105

DOSAGE: greater than 150 mg.

DURATION: unknown.

QUALITATIVE COMMENTS: (with 150 mg) No effects whatsoever.

(with 150 mg) The effects, if any, were so-so. Perhaps a threshold. But my libido was non-existent for three days.

(with 550 mg) I took 550 milligrams of it Saturday night and I had a pretty bad trip. On a scale of positive 10 to negative 10 it was about a negative 6. It really downed me. Two other friends took 200 milligrams. They found it very pleasant after about 20 minutes. It was a plus 3 [on the -10 to +10 scale]. Then it wore off a little bit; and then, 4 hours later, it hit them even stronger and was about a plus 5.

(with 1000 mg) I took up to a gram of it and absolutely nothing.
 
i suppose the mercury is in salt form so will give a higher boiling point anyway. both oes and ms r possible. how much mercury is used to produce how much product? the reason i ask is i can, without appearing dodgy is to get 4( tested by the same icp) 10gm fine soil samples with no mercury in, add a finely crushed pill to one sample and get all four analysed. just worrying about the dilution factor, as i don't imagine there would that much Hg used in this process. dos that make sense? suggestions?
 
Very little is used, usually in the form of Mercury (II) chloride. It's more a contamination problem that's the issue, but it would be an interesting exercise nonetheless.

It would also be important to stress that results of a few pills (which would likely be negative) does not mean any and all pills are guaranteed mercury free.

Of course, as you know you'll need to use ICPMS with Hg. Assuming no accidental contamination, if any is present, and that of course will likely only be the case if HgCl2/Al amalgam was used in reductive amination, then levels will probably only be in the order of ppt.
 
So we r not talking about residual Hg from the reaction but carelessness by the chemist.(spills etc.)? I'm not sure that ms reads at ppt and if it does our instruments r not calibrated 4 such detection limit. won't be a drama getting the assay(ppb) done, always a drama getting samples though. slim pickings 4 me.bear with me on this point. will try as soon as i can get samples. One day i hope the powers that be actually care enough to provide testing 4 us. wishful thinking perhaps. Anyway, i'll let y'all know how it goes.
 
haribo1 said:
From my knowledge, the most common methods are either hydrogenation using methylamine gas & catalyst (large scale) or the 'cold method' using NaBH4 with CH3NH2 in methanol. The cold method can be carried out in any handly vessel & can be done by a trained chimp. I've seen a lot of stuff made in The Netherlands and I've never seen the leuckard method used. Why would you? It's messy, smelly and uses a chemical even MORE watched than methyl amine (the PMK is a given).
Oh, and hobbiests use the Mercury amalgam method since it's handy for kitchen sink scale.
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you are right for mdma production, but still a lot of amphetamine labs in .NL use the leuckart method according to annual reports of the dutch police.
don't have the most recent reports, so don't know if this info is still valid.
 
So we r not talking about residual Hg from the reaction but carelessness by the chemist.(spills etc.)? I'm not sure that ms reads at ppt and if it does our instruments r not calibrated 4 such detection limit.
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Well, if the Hg salt was used, due to the slight solubility in non-polar mediums, there will theoretically be some residual Hg left. It may be in slightly higher amounts depending upon how much was used, but in reality the danger would be greatest when lab techniques aren't up to scatch i.e. failure to do the crystallisation in the correct medium, contamination from dirty vessels etc.

It may very well be that levels could be present in the ppb range, so I'd still think it's worthwhile doing such a test. Of course, the MDMA in the samples could have been produced via another reduction method, either borohydride or H2/catalyst etc. in which case there would be no mercury present.

won't be a drama getting the assay(ppb) done, always a drama getting samples though. slim pickings 4 me.bear with me on this point.
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We'll be as patient as you need us to be :)
 
I love, Febuarys report!

That polydrug seizure is fucking insane, all that acid gone to waste is just a tradgedy. . . . . looks at the ground in silence.

And right at the bottom they have an open position to analyze all those goodies for the DEA, Awesome!
 
Analysis by color testing, GC/MS, FTIR/ATR, and microcrystal test indicated MDMA, nicotinamide (not confirmed), trace MDP2P, and trace methamphetamine. The exhibits were not quantitated, but the ratio of MDMA to nicotinamide was 37:2 based on the TIC. This is the first submission of Ecstasy tablets with glitter (and also of this logo type) to the laboratory.
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P_d? :) MDP2P....
 
i wonder if they can trace origin by the glitter like what csi does on tv lol. A great read :)
 
ppt levels of Hg?

I can see down to 100 ppt on the instrument in my lab. Cold Vapor Atomic Absorption. Atomic fluorescence can go even lower.

I think the poster who said it was likely carelessness in the lab, rather than residual Hg remaining from the synthesis, was right on. Al amalgam reactions are done in a very strongly reducing environment, and Hg is a pretty noble metal.
 
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Thanks for posting, I've been meaning to catch up on my Microgram reading for a while :)
 
This little gem was the among the best reading for me.

12. Sarwar M. A new, highly specific color test for ketamine. Microgram Journal 2006;4(1-4):24. [Editor’s Notes: Treatment of ketamine with alkaline gold bromide produces a deep purple color within approximately one minute that changes to dark, blackish‑purple within approximately two minutes. The color, color change, and time frames constitutes a highly specific screening test for ketamine. The test is negative for amphetamine, methamphetamine, MDA, MDMA, and PCP, all of which are occasionally encountered in combination with ketamine. Contact: Forensic Research Laboratory, Center for Excellence in Molecular Biology, University of the Punjab, Lahore, Pakistan.]
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Gold bromide isn't that expensive, although a reagent kit would certainly cost more than currently available tests. Pity it wasn't discovered a few years ago when ketamine was a common MDMA substitute.
 
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