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Author: Subject: What is wrong with MDMA production nowdays?
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[*] posted on 25-1-2020 at 17:07


Quote: Originally posted by karlos³  
What atara says has hand and feet.
It is not MDMA what you see on the other NMR, it is another substance, likely the 3,4-dimethoxymethamphetamine he suggested.


Aye even the nmr tester said that.. but look at NMR #3 MDMAnmr... that was the FIRST NMR that started this whole thing and is closer to MDMA ;)

We had magic sample, sample A and sample B...

Sample A was MDP2-pol and MDMA but we can't find the NMR and we cant sample it anymore. We are trying to find it thou...

At this point we need a lot more Meh and magic samples
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[*] posted on 25-1-2020 at 17:30


Hm, no, the BDO peak is at 5.97. That makes water contamination more likely to explain the 4.87.

See:

http://www.scielo.br/scielo.php?pid=S0103-50532018000901944&...

But both of the "wrong" batches still have a large unexplained peak around 3.5-3.7. The "good" batch has only small peaks in this region. In the batch you claim was synthesized by a trustworthy lab this peak is at 3.489 and in the other bad batch it's 3.696.




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 25-1-2020 at 17:32


Quote: Originally posted by clearly_not_atara  
Hm, no, the BDO peak is at 5.97. That makes water contamination more likely to explain the 4.87.

See:

http://www.scielo.br/scielo.php?pid=S0103-50532018000901944&...

But both of the "wrong" batches still have a large unexplained peak around 3.5-3.7. The "good" batch has only small peaks in this region. In the batch you claim was synthesized by a trustworthy lab this peak is at 3.489 and in the other bad batch it's 3.696.


Correct both of the "wrong" batches still have a large unexplained peak around 3.5-3.7 is about all we got so far. We are hoping for more info soon. But without more batches of meh and magic it is hard to go on. Sadly my exp is MDMA synthesis not NMR sadly. I only know someone with access to an NMR which has helped immensely

[Edited on 26-1-2020 by pastor]
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[*] posted on 25-1-2020 at 18:04


Unfortunately just about every fg potentially has a peak there :D

If I didn't know better I'd say it was free radical oxidation creating an -OH somewhere... but the likely products either a: are active (the N and the methyl), b: give radically different GCMS (anywhere on the propane/ring) or c: give radically different NMR (the methylene).

Another possibility is that the MDMA contains some proportion of 3,4-methylenedioxy-2-propanol. This would result from a failed synthesis, but again I'd be surprised it didn't come up on a GC/MS... it might be colorimetrically invisible since it's largely non-nucleophilic




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 25-1-2020 at 18:19


Quote: Originally posted by clearly_not_atara  
Unfortunately just about every fg potentially has a peak there :D

If I didn't know better I'd say it was free radical oxidation creating an -OH somewhere... but the likely products either a: are active (the N and the methyl), b: give radically different GCMS (anywhere on the propane/ring) or c: give radically different NMR (the methylene).

Another possibility is that the MDMA contains some proportion of 3,4-methylenedioxy-2-propanol. This would result from a failed synthesis, but again I'd be surprised it didn't come up on a GC/MS... it might be colorimetrically invisible since it's largely non-nucleophilic


We did have one batch of POL (tested via drugs data and came back 1:5 I think? ) and we tested it via nmr but We can't find that report sadly.
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[*] posted on 25-1-2020 at 18:44


Quote: Originally posted by clearly_not_atara  
Unfortunately just about every fg potentially has a peak there :D

If I didn't know better I'd say it was free radical oxidation creating an -OH somewhere... but the likely products either a: are active (the N and the methyl), b: give radically different GCMS (anywhere on the propane/ring) or c: give radically different NMR (the methylene).

Another possibility is that the MDMA contains some proportion of 3,4-methylenedioxy-2-propanol. This would result from a failed synthesis, but again I'd be surprised it didn't come up on a GC/MS... it might be colorimetrically invisible since it's largely non-nucleophilic


I know the trustworthy lab route was safrole, MDP2P via MEOH BENZ wacker... AL/HG. But no pol was detected via GC/MS when we did it... batch MDMAnmr. WHATever "it" is has the same mol weight of MDMA and passes reagents MMMS

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]
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[*] posted on 25-1-2020 at 21:14


I'm going to go out on a limb here and say that this is a pretty fruitless endeavour of yours, pastor.

If you claim to be about harm reduction, you now have ample evidence that there is no quality control and there could be any amount of unidentifiable junk in what passes for an ecstasy tab. You can now make a pretty good case that people are shelling out cash for unknown swill and it is just as likely to be hazardous as it is to be ineffective.

You seem to overlook the fact that MDMA and its chemical cousins are prohibited substances in pretty much every country and with good reason. People die using this stuff. And countless more have their lives ruined by it.

It would be a better policy to steer people away from this stuff than to make such haphazard and unsystematic efforts in identification of random crap.
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[*] posted on 25-1-2020 at 23:41


Quote: Originally posted by j_sum1  
I'm going to go out on a limb here and say that this is a pretty fruitless endeavour of yours, pastor.

If you claim to be about harm reduction, you now have ample evidence that there is no quality control and there could be any amount of unidentifiable junk in what passes for an ecstasy tab. You can now make a pretty good case that people are shelling out cash for unknown swill and it is just as likely to be hazardous as it is to be ineffective.

You seem to overlook the fact that MDMA and its chemical cousins are prohibited substances in pretty much every country and with good reason. People die using this stuff. And countless more have their lives ruined by it.

It would be a better policy to steer people away from this stuff than to make such haphazard and unsystematic efforts in identification of random crap.


Well these tests are DETECTING differences. Much more so then GC/MS. ANd deter people. You know these people are. My CrYsTaL TuRnS StRiAgHT To BlAcK aNd EC Says 97%... Good luck telling those people. Even getting people to admit ALL MDMA on CG/MS is not equal is like pulling hairs getting ANYONE to believe us, hence the post here. Getting people to admit we have a difference between most old market vs new market MDMA, cuz us old times did too much MDMA... RIGHT..

We believe it is possibly caused by a lack a methylamine and or failure to distill the freebase before gassing. We will need more samples, which we are procuring and we do have someone reading the NMR in depth. At this point it's all data driven and we need more data!!! But we are finding patterns

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]
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[*] posted on 26-1-2020 at 04:26


Quote: Originally posted by pastor  
At this point it's all data driven and we need more data!!! But we are finding patterns


At this point i think you grossly overestimate everybody else's interest in figuring this out.

Why don't you just make sure you start with clean and proper materials instead of trying to crowdsource knowledge about what went wrong with your cooking? There is no mystery to this: Either you put in shit or you done shit. Solved.

Established synthetic pathways reproducibly give correct products. Whatever went wrong with yours, who knows and who cares?
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[*] posted on 26-1-2020 at 07:45


I agree with SS that the title is invalid. There are plenty of people myself included who have had magical experiences on MDMA synthesized in this decade.

A better question might be “why do some batches of MDMA seem to be unusually weak?”. In this framing there is the potential for contamination by some inactive impurities such as MDP2Pol, N,N-dimethyl-MDA, occurring rarely.




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 26-1-2020 at 08:00


I'd bet money that spectrum "...207" was run in methanol. The unlabeled peak at 3.31 corresponds to the solvent residual signal of methanol, and there is always a lot of water present in deuterated methanol if it's been opened before. That big 4.87 peak is exactly where water shows up in methanol. If D2O was the solvent it would be seen around 4.79. So there's nothing amiss with that sample, it is reasonably pure.

The other one does look like it was done in D2O (presumably as the HCl salt) albeit maybe not properly referenced. I'm not sure why the multiplet around 3.3 is not integrated. That should correspond to the proton on the tertiary carbon. If you consider that, then there must be some spurious junk in the peak around 2.5 that is integrated as 5 (should come out to 4), plus there's that quartet at 3.38. A quartet often implies an ethyl group.

I'm not too familiar with potential impurities that may be present, so I won't go out on a limb to guess at what could be in there, especially since it's hard to see what exactly is going on in that 2.5 peak. Having the original raw data to look at more closely in Topspin would be nice. Barring that all I can say is that your "meh" stuff does indeed look "meh."




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[*] posted on 26-1-2020 at 09:09


Quote: Originally posted by stoichiometric_steve  
Quote: Originally posted by pastor  
At this point it's all data driven and we need more data!!! But we are finding patterns


At this point i think you grossly overestimate everybody else's interest in figuring this out.

Why don't you just make sure you start with clean and proper materials instead of trying to crowdsource knowledge about what went wrong with your cooking? There is no mystery to this: Either you put in shit or you done shit. Solved.


Established synthetic pathways reproducibly give correct products. Whatever went wrong with yours, who knows and who cares?


BECAUSE, my lab is one thing... That can easily be fixed, we can reun with excess of methylamine, ran a DMF wacker vs MEOH, etc, etc ... BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high, needs 200+mg to feel ANYTHING and even then they don't smack unlike the 80-120mg of yesteryear. We aren't trying to fix my batch. We are trying to fix the WORLD MARKETS OF MDMA.

Hopefully someone in the clandestine scene will listen to us when we do find the issue, but this isn't about fixing "our product" That is as simple as rerunning our batch or doing a different animation... No we are trying to fix the world's supply for the most part. Why are SO MANY labs are creating meh and where/why did all the magic go. Hence the large effort on bluelight, why we want to find out the issue, the impurity/s and how we can clean it and turn meh into active magic. Either by means of middle men cleaning bulk product via column or recrystallization. We want to find out the most common causes/issues so we can clean product, and why so many dutch superlabs seem to be making meh.

My guess is PROBABLY happening during animation but that is all I have to go on.


[Edited on 26-1-2020 by pastor]



[Edited on 26-1-2020 by pastor]
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[*] posted on 26-1-2020 at 09:58


The only difference between the old stuf you are speaking of and the nowadays is the precursor the MDP2P is derrived, but i cant find what that a big difference can make, have had some stuff that isnt produced from glycidate and it rocks have had some stuff that is from the DNM and i just consider it cutet as a higher dosage was needed for the same results but i dont get your problem MDMA still is almost number 1 choise of drug users who want to rave, so shurely the magic is still there...

[Edited on 26-1-2020 by dextro88]
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[*] posted on 26-1-2020 at 10:37


Quote: Originally posted by dextro88  
The only difference between the old stuf you are speaking of and the nowadays is the precursor the MDP2P is derrived, but i cant find what that a big difference can make, have had some stuff that isnt produced from glycidate and it rocks have had some stuff that is from the DNM and i just consider it cutet as a higher dosage was needed for the same results but i dont get your problem MDMA still is almost number 1 choise of drug users who want to rave, so shurely the magic is still there...

[Edited on 26-1-2020 by dextro88]


Our private lab batch WAS SAFROLE and reductive animation was Al/Hg. SO it is not Glycidate vs safrole debate that flew out the window with NMR analysis #1... And yes, I have a batch of MAGIC from a burning man source not darknet so it's more "family" product. People on the hive in 1997-04 complained of inactive/meh product as well from safrole, it just wasn't as common. If you read the all the bluelight pages you'll find a few reports

You are missing that Reductive amination process also changed from lukehart and Al/Hg to catalytic hydrogenation via platinum, adams catalyst or H2 for yield/purity... Borohydrides are slow for clandestine on the dutch scale. While i'm sure the lukehart MDA/MDMA had something to do with SOME of the old magic... It is def not indicative of the magic that floats around now. Also I see a LOT more MEH than magic and it's fooling Energy control Darknet avengers MDMA testing. That is for sure.

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]
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[*] posted on 26-1-2020 at 10:53


So here's my rationale for MDP2Pol and/or N,N-dimethyl-MDA (MDDM) appearing as synthetic impurities in MDMA synthesized by reductive amination of MDP2P with MeNO2 under acidic conditions:

- direct reduction of the ketone leads to MDP2Pol, this should be unlikely but may occur with excessively high temps / too much reducing agent

- the Nef reaction on MeNO2 generates formaldehyde, which may reductively aminate MDMA to MDDM.

But neither possibility acceptably explains the 3.5-3.7 peak.

There is another peak that changes in the good sample relative to the "meh" samples, around 2.7. The "meh" samples have peaks around 2.55-2.59 but the good one is at 2.71. This shift is small but it could be meaningful. Published NMR spectra of MDMA tell me that this peak is typically located on the N-methyl group and furthermore that it should be at 2.7, which does suggest that we're getting somewhere.

In fact, since the NH proton apparently does not appear in the NMR spectrum (can someone confirm?), I think this shift could be consistent with double N-methylation leading to MDDM impurities.

Reference NMR attached.

mdma_nmr.jpg - 179kB




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 26-1-2020 at 11:15


Quote: Originally posted by clearly_not_atara  
So here's my rationale for MDP2Pol and/or N,N-dimethyl-MDA (MDDM) appearing as synthetic impurities in MDMA synthesized by reductive amination of MDP2P with MeNO2 under acidic conditions:

- direct reduction of the ketone leads to MDP2Pol, this should be unlikely but may occur with excessively high temps / too much reducing agent

- the Nef reaction on MeNO2 generates formaldehyde, which may reductively aminate MDMA to MDDM.

But neither possibility acceptably explains the 3.5-3.7 peak.

There is another peak that changes in the good sample relative to the "meh" samples, around 2.7. The "meh" samples have peaks around 2.55-2.59 but the good one is at 2.71. This shift is small but it could be meaningful. Published NMR spectra of MDMA tell me that this peak is typically located on the N-methyl group and furthermore that it should be at 2.7, which does suggest that we're getting somewhere.

In fact, since the NH proton apparently does not appear in the NMR spectrum (can someone confirm?), I think this shift could be consistent with double N-methylation leading to MDDM impurities.

Reference NMR attached.


He made and purified the methylamine from I believe hexamine and did not use nitromethane. Nitromethane was not used at all. AT least this is what I know from our private lab MDMAnmr batch made from safrole. I think he did say his mantle has having temp swings, which could also make sense of MDDM...

I do not know if you are implying about meh batch 1 or 2... If it helps MDMAnmr #1 a uvspot test was done yesterday. Shows there is only 1 compound. It showed there was an amine and there are no other amines active or not. He stained the TLC with ninhydrin. I can upload the plates UV and non UV later if you want

PS thank you for everyone who has taken the time to lookover our NMR reports and while some people think we are crazy, there is something happening on a scale that we would like to figure out :)



[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]
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[*] posted on 26-1-2020 at 11:32
KEWL


This is turning into a KEWL place!

Great. Go to burning man. Get stoned out of your mind
and fry some brain cells.

If that aint KEWL, I don't know what is!:o




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[*] posted on 26-1-2020 at 11:53


Quote: Originally posted by sodium_stearate  
This is turning into a KEWL place!

Great. Go to burning man. Get stoned out of your mind
and fry some brain cells.

If that aint KEWL, I don't know what is!:o


Some people don't DO drugs but find MDMA synthesis interesting, some people find lab analysis interesting, some people only sell drugs and want to have quality product for their clients. Regardless we had someone look at NMR analysis #1 and he said on the surface the MDMA appears to be MDMA . If you don't find it interesting or COOL or interesting that GC/MS is being fooled and fooling Energy control, Drugs data and private labs (friend who has access to NMR) Then this conversation isn't for you.

If you do find it interesting that GC/MS , MALDI, UltraViolet–Visible Spectroscopy and other tests are being fooled then please join the conversation in a positive manner :) We are not discussing MDMA synthesis which is against forums rules, but why and how reliable are these tests in the first place. At least 1 or 2 people find it interesting and are willing to contribute in a positive manner or light for one reason or another.

[Edited on 26-1-2020 by pastor]
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[*] posted on 26-1-2020 at 12:19


Quote:
He made and purified the methylamine from I believe hexamine and did not use nitromethane. Nitromethane was not used at all. AT least this is what I know from our private lab MDMAnmr batch made from safrole. I think he did say his mantle has having temp swings, which could also make sense of MDDM...


How do you know this? How can you respond so quickly about a synthesis that someone else carried out years ago?

Quote:
If it helps MDMAnmr #1 a uvspot test was done yesterday. Shows there is only 1 compound. It showed there was an amine and there are no other amines active or not. He stained the TLC with ninhydrin. I can upload the plates UV and non UV later if you want


Ninhydrin does not react with MDDM or other tertiary amines

Quote:
BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high


This is simply false. Again, it contradicts the experiences of thousands of people who get high just fine

[Edited on 26-1-2020 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 26-1-2020 at 12:21


Quote: Originally posted by pastor  
We aren't trying to fix my batch. We are trying to fix the WORLD MARKETS OF MDMA.



We want to find out the most common causes/issues so we can clean product, and why so many dutch superlabs seem to be making meh.


Why would ANYONE here help out ORGANIZED CRIME who apparently "don't know how to cook their shit"?

Do you know what's really wrong with them? They cook whatever shit it takes to make money, not to give you magical experiences. Nobody gives a shit about you or your drug buddies or your trips. For all they care, after you give them all your money, you can die in a ditch.

The only thing you can and should do is rally for controlled legalization.
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[*] posted on 26-1-2020 at 12:22


Quote: Originally posted by stoichiometric_steve  


Why would ANYONE here help out ORGANIZED CRIME who apparently "don't know how to cook their shit"?


Look man I don't know if this is still a chemistry forum but I find the NMR discrepancies interesting. We have three batches, one good, two bad, and some correlations.




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 26-1-2020 at 12:43


Quote: Originally posted by clearly_not_atara  
Quote:
He made and purified the methylamine from I believe hexamine and did not use nitromethane. Nitromethane was not used at all. AT least this is what I know from our private lab MDMAnmr batch made from safrole. I think he did say his mantle has having temp swings, which could also make sense of MDDM...


How do you know this? How can you respond so quickly about a synthesis that someone else carried out years ago?

Quote:
If it helps MDMAnmr #1 a uvspot test was done yesterday. Shows there is only 1 compound. It showed there was an amine and there are no other amines active or not. He stained the TLC with ninhydrin. I can upload the plates UV and non UV later if you want


Ninhydrin does not react with MDDM or other tertiary amines

Quote:
BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high


This is simply false. Again, it contradicts the experiences of thousands of people who get high just fine

[Edited on 26-1-2020 by clearly_not_atara]


Ah good question, you see the batch was made Oct 28th of 2019, arrived halloween day with me and a DRUG virgin who has only done small amounts of cocaine. She did not roll until after 250+ to 350mg. The product was then tested nov. 18th via NMR via another friend after he ran GC/MS and MALDI came up positive for MDMA thou he SWORE up and down 97% via GC/MS and MALDI confirmation. I asked did you get high he was like no not really, then thus then he ran a NMR

I know the route because I was in contact with the person as The source of safrole was provided by me, it is still QUITE COMMON in 2019/2020 in the USA if one looks hard enough... my results via analysis show it is still QUITE available without any regulation if you look the correct way. (no i'm not gonna tell anyone go away) and @stoichiometric_steve I only gave him a VERY small amount of safrole... like 2 to 3 oz yeez. Some kingpin you make me out to be


Anyways he also detailed the route via messages and I could go back anytime, thou it would be a huge pain the way we kept in contact. Hence why/how I know so much and can respond so quick it's only been 2.5 months . And he made it from Formaldehyde + Ammonium Chloride not hexamine my bad close enough thou to exclude nitroethane. He followed brightstar according to my records but made his own p-Benzoquinone from hydroquinone . I even remember the picture of p-Benzoquinone he made. The product was acetone washed 2-3 times, but was not recrystallized.



Also while magic is still around (I have recently bought some, If you search bluelight everyone is asking which darknet dealer has magic and no one seems to have an answer but that's just what I know) My last 3-4 dealings on the darknet have been MEH and I haven't got magic online in ages but I haven't bought online since like 2017/18. Maybe i'm wrong, magic does exist but even my own supplier has issues finding someone with good stuff.

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Yeah, extremely rare, if not impossible, to find MDMA that looks like that on the DN. I’ve been buying exclusively from markets for the past 3 years and have never come across any.

Others may have had better luck than me though. see thread

https://www.bluelight.org/xf/threads/what-is-wrong-with-the-...


There are variations of the MEH stuff some active at 200-250mg, But your not rolling , it doesn't come in "waves" , you need at least 200 mg to feel something, Your pupils are not saucers, You do not sweat super easy.Yes you can feel the meh stuff and it canget you high, of course but oldtimers can tell a difference, from time to time a batch of magic does come thru but from my experience most darknet MDMA is meh, along with people's exp on bluelight. Does magic active stuff exist yes, have I found it, yes but I think for every 1 good batch is around 5 bad batches (norcal molly scene most people at least reagent test here) , a good example is when I look at my local rave scene. People on this "new stuff" zone out and are zombies/lethargic. They lack any energy. This is from my exp at local renegades where it's a more family scene, I avoid big shows and only go to the hippy music festivals. I'm not sure what your guys exp with MDMA is but enough reports are coming in that SOMETHING is causing a huge issue and people taking 300-500mg in a night is a HUGE nono. I use to think MDMA is MDMA, A result Frpm energy Control of MDMA is MDMA then I got this meh batch and my view 100% changed. NMR's seem to confirm that and Maldi and GC/MS is not accurate it appears. We can't explain what MEH feel like only that people new to MDMA think it's MDMA but something is off/dulled. It will get people high just 200mg doesnt make you roll tits like 80-120mg of magic will that's all I have to say about that in mine and others experiences of the current markets in our area.




[Edited on 27-1-2020 by pastor]
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[*] posted on 26-1-2020 at 13:50
Dain Bramage


What would happen if these samples were tested
by an independent lab, by qualified research chemists
that are not users of the substance being tested?

My theory is that they'd find the answer.:D




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pastor
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[*] posted on 26-1-2020 at 14:00


Quote: Originally posted by sodium_stearate  
What would happen if these samples were tested
by an independent lab, by qualified research chemists
that are not users of the substance being tested?

My theory is that they'd find the answer.:D


Sadly almost noone has access to an NMR, and to be fair he has only sampled 1 of the 3 NMR samples that was meh sample 1. Reading NMR is not his strong suit he just works in a lab with access to one. We have someone else attempting to reading them on bluelight but he has been busy and wants to read the report correctly. We did post here to get more people involved thou as to speculate what is wrong. AT least 1 person finds it interesting so I give it that.

I remember about oh 4-5 years I remember a darknet vendor called caslava, he had a $10k bitcoin bounty on his xanax to disprove his 99.X % pharma purity. I wish I had access to NMR back then lmao. I only met someone last year with one. And trust me I ASKED.... WHen asked why he wouldn't take an energy control GC/MS he said it was garbage. These MDMA samples pretty much confirm our suspicion about that. Also I sent xanax powder that looked like crushed pills and had no bitter xanax taste, Energy control said 99% xanax even thou clearly not true. Hence My understading of Caslava hating GC/MS




[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]
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G-Coupled
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[*] posted on 26-1-2020 at 15:00


Was the crushed powder active at all when ingested? I wonder what it could've been?

Are all GC/MS analyses created equal? I don't mean screwing up the procedure (although I'm sure that happens plenty), more like do all the devices produce pretty much the same data given a particular sample?

Are the different models of GC/MS significantly different from one another? Do we know which machines Energy Control might be using?

[Edited on 26-1-2020 by G-Coupled]
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