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Amphetamine Sulfate Cleanup Options
 
DrSeltsam
#1 Posted : 5/22/2018 9:06:16 PM

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Dear fellow Nexians,

Mostly out of scientific curiosity, I would like to do a cleanup of Amphetamine. It is something I would like to do for a friend (as my interest in this stuff is very limited) and I don't know the source of the substance. I suspect it to be cut as hell and thus would like to clean it. I would do the following procedure:

1.) Wash with dry acetone until the acetone comes out clear
2.) Dissolve in a minimum amount of dH20, and make acid with some vinegar
3.) Wash with d-limonene twice
4.) Basify and extract three times with d-limonene
5.) Pool the NPS, wash once with brine, and dry over MgSO4
6.) Prepare a solution on food grade H3PO4 in acetone and try over MgSO4 and add this to the d-limonene until no more substance crashes out
7.) Filter and dissolve in dH2O, evaporate the water quickly to remove the rest of the d-limonene

What do you guys think? Should work, shouldn't it?

Thanks!
 

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Mindlusion
#2 Posted : 5/23/2018 1:15:59 AM

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you should edit your post and remove any mention of procurement.

That clean up would do the trick, but I would not recommend using H3PO4. It is unlikely you will obtain good crystals. I would stick to HCl or H2SO4 in this case.

You could also try simple recrystallization, dissolve in boiling IPA or ethanol, decant from the insolubles, allow to cool to room temp for crystallization.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
CosmicLion
#3 Posted : 5/23/2018 1:19:16 AM

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Not to be a party pooper... and I don't like being the first one to say it...

But this community frowns upon amphetamine abuse, I doubt you will find TOO much support for it here...

If it is "amphetamine" and not "methamphetamine" just get a prescription.... it's not hard and you will know it is pure... and insurance will likely pay for it.

Problem solved...

Be careful, I don't know your experience with the stuff, but even plain "amphetamine" can cause long term damage to your dopamine systems.

You are truly taking from your future to gain something in the present and it is almost guaranteed with any kind of regular use... that you will regret it later in life.

Stay safe! Thumbs up
-Eternally Romping the Astral Savannahlands-
 
CosmicLion
#4 Posted : 5/23/2018 1:27:16 AM

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Just adding on to my comment...

I've seen it among friends, family members, fellow students, and patients I've seen working in the medical industry for 17 years... Unless they are just taking it daily for years/decades on end, they almost unanimously agree it was a mistake and suffer after-effects years after discontinuing use.

No judgements... The stuff makes you happy, and you can get a lot done... Totally understandable why you are drawn to it...

Just giving you a heads up for your own benefit..

Love Thumbs up
-Eternally Romping the Astral Savannahlands-
 
DrSeltsam
#5 Posted : 5/23/2018 8:20:02 AM

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Mindlusion, thanks for the hint. I edited my post and put the truth (and I am not joking).

Regarding using H2SO4: This will work, of course, but I can't source food grade/pharma grade H2SO4. Going for technical qulity would be an option but I would consider H3PO4 superior in this case.

Using HCl: The HCl salt is highly hydroscopic and thus not stable. I looked in old books for pharmacist and only the sulfate and the phosphate salts are described. This is also confirmed by this discussion.

Regarding recrystallisation: acetone or IPA seems unpractical to me as I would never know if the remaining part is just substance which didn't dissolve yet or cuttings like sugars. Thus, it is very hard to know when to decant of the rest.

CosmicLion, thanks for your effort to warn me about the substance and the long-term harm that might come from abusing it. I appreciate that you take your time to warn me.

I am not particularly drawn to amphetamine. In fact I never consumed it. It's mainly curiosity if I can do the cleanup and a favour for a friend. I am not even sure if I would consume it. I have enough energy myself, I am happy with were I am with life currently, and don't overdo things.

A prescription is not an option. Where I live, you would get methylphenidat and even this is hard, very hard. Not all countries are like the US Pleased
 
Cactus Man
#6 Posted : 6/2/2018 5:27:47 AM
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Alkaloids over amphetamines Thumbs up
 
endlessness
#7 Posted : 6/2/2018 5:51:46 PM

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Cactus Man wrote:
Alkaloids over amphetamines Thumbs up


Amphetamines are alkaloids too Smile

Not the ones im interested in though, neither the focus of the Nexus.

Either way for harm reduction's sake I find it a legitimate question to ask and be answered, as an isolated thread here.

DrSeltsam, most amphetamine (70%+) is cut with caffeine, which I think might still make it through your clean up plan, not sure though would have to check for caffeine solubility in those solvents. Anyways caffeine is not worrysome health-wise

Sometimes amphetamine has DPIA which is a synthesis impurity, of unknown health risks and i'm unsure of solubility too.

Occasionaly you also find n-formylamphetamine, another synthesis impurity.

Other products you find like solvent traces and inactive salts from synthesis are: phenylacetone, calcium sulfate, isopropanol, methanol, ethylenglycol

These are the main compounds found in amphetamine (source 1, source 2 ), so it gives you somewhere to start in regards to looking into solubilities and ways of cleaning them.

I also recommend at least reagent testing, or better TLC testing, to make sure you have indeed amphetamine and not something else entirely (for example 2-FA or another RC of unknown safety profile), or to confirm your clean up is working.
 
DrSeltsam
#8 Posted : 6/6/2018 3:59:51 PM

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Hi endlessnes,

Thanks for your reply!

The acetone wash and washing the dissolved powder with a NPS will remove caffeine. Normally, the acetone wash alone should remove caffeine but the second step with the NPS should get everything.

I don't think this cleanup will reliably remove impurities like DPIA or n-formylamphetamine. They are too similar to amphetamine and will probably remain. To do this, you would need to vacuum distill or do a column chromatography. All other things, like phenylacetone, calcium sulfate, isopropanol, methanol, ethylenglycol, etc., will be removed or evaporate in the process.

Testing goes without saying that this does not substitute testing Smile
 
Mindlusion
#9 Posted : 6/6/2018 4:50:58 PM

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Re-crystallization is the only reliable way to remove the impurities. Washing is only effective post-recrystallization because you are washing out the recrystallization solvent which contains the impurities. If you don't recrystallize, washing is ineffective since the impurities are trapped within the solids.

The beauty of re-crystallization is that, as long as your sample is relatively concentrated in amphetamine (>80%) in most cases crystallization will be selective to the amphetamine, or whatever the dominant product is, regardless of polarity, solubility, etc. You should be able to very easily get a product of >99% by re-crystallization only, no column chromatography or distillation necessary.

Of course, what would be even better is to an acid/base workup extraction and resalting prior to recrystallization.

It is pretty easy to tell what is product and what isn't, don't let that put you off. The salt is also extremely soluble in boiling IPA, so per say 1g, anything that doesn't dissolve in 15mL boiling IPA is junk, and that is probably still a generous amount of IPA. You can always save it and try to dissolve it again before throwing it out.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
DrSeltsam
#10 Posted : 6/8/2018 9:06:20 AM

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Mindlusion, thanks a lot for your reply and the comments.

From what I found on mdma.ch, recrystallization is very hard for the sulfate salt and only really possible from dH20 (which immense losses) (source). Do you know for sure that this works?

If yes, I would revise the procedure to:

1.) Wash with dry acetone until the acetone comes out clear (this will remove the caffeine cuts and bring the purity up for the next step)
2.) Recrystallise from dry IPA and filter if necessary
3.) Wash with acetone again to clean the surface.

Thanks a lot!
 
DrSeltsam
#11 Posted : 6/18/2018 8:37:46 AM

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This is what I have done:

Air-dried the stuff (strong smell of phenylacetone and other solvents).
Washed with dry acetone several times. After evaporating the acetone, only an oil with a sweet smell was left.
Dissolved in dH2O and evaporated the liquid in a pot. What was left was not smelly anymore and reacted as it should to a marquis test.

Until here I lost 75% of the initial weight.

I put the substance in a paper bag and put it in a box with dry MgSO4 for several days to ensure that it was try. Then I tried to recrystallise from dry IPA. I tried to add the IPA bit by bit until I reached 25 ml for 1.2 g. No significant amount went into solution after 10 minutes of boiling. I'm not sure if one can do this from IPA alone....
 
DrSeltsam
#12 Posted : 7/15/2018 4:28:17 PM

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Some update:
at a festival I took advantage off the drug checking program they offered there.

The white stuff described above is 90% amphetamine. They couldn't tell me what the remaining 10% were but it shouldn't be harmful.

I did the math and I guess that by dissolving it in water and evaporating the water again I might produced the monohydrate. The monohydrate would be 10% heavier and usual gcs would not detect the water (we had the same case with mescaline sulfate in this forum).

At least we figured out that one can not do a recrystallization of amphetamine sulfate from IPA.
 
blue.magic
#13 Posted : 5/25/2019 8:09:53 PM

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I have an opporutnity to obtain chemically pure DL-amphetamine sulfate, so I will do experimentation and try the re-x with various alcohols. People gave me samples in the past to do the reagent test and TLC and more often than not, the cut samples didn't dissolve completely (presence cutting agents). So this might have been your case.

Monohydrate might be preferable over anhydrous form because of weight stability.

So far from what I read (various forums), IPA should work just fine, but you have to use enough of it and near-boiling. Anhydrous ethanol and methanol might work better (less solvnet needed).

I've read some poeple use ethanol/acetone system for dual solvent recrystallization, but I haven't found any information about the qunatities used.

According SWDRUG monograph:

Quote:
Dissolve the sample in water and add 0.1 N sodium hydroxide until basic. Extract the amphetamine base from
the aqueous layer with hexane. Filter the hexane extract through a bed of anhydrous sodium sulfate. Bubble
HCl gas through the hexane to form the hydrochloride salt.


Unfortunately, sulfuric acid cannot be used as it reacts with hexane.

What could work after this A/B extraction, is to remove the solvent (hexane) under vacuum, dissolve your amphetamine sulfate in dry IPA, filter, add - dropwise - sulfuric acid in IPA (50% or so). The salt should drop out of solution and what remains is to filter and dry the solids.
 
Cactus Man
#14 Posted : 5/25/2019 9:12:19 PM
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endlessness wrote:
Cactus Man wrote:
Alkaloids over amphetamines Thumbs up


Amphetamines are alkaloids too Smile

Not the ones im interested in though, neither the focus of the Nexus.

Either way for harm reduction's sake I find it a legitimate question to ask and be answered, as an isolated thread here.

DrSeltsam, most amphetamine (70%+) is cut with caffeine, which I think might still make it through your clean up plan, not sure though would have to check for caffeine solubility in those solvents. Anyways caffeine is not worrysome health-wise

Sometimes amphetamine has DPIA which is a synthesis impurity, of unknown health risks and i'm unsure of solubility too.

Occasionaly you also find n-formylamphetamine, another synthesis impurity.

Other products you find like solvent traces and inactive salts from synthesis are: phenylacetone, calcium sulfate, isopropanol, methanol, ethylenglycol

These are the main compounds found in amphetamine (source 1, source 2 ), so it gives you somewhere to start in regards to looking into solubilities and ways of cleaning them.

I also recommend at least reagent testing, or better TLC testing, to make sure you have indeed amphetamine and not something else entirely (for example 2-FA or another RC of unknown safety profile), or to confirm your clean up is working.


my ignorance of all things related to amphetamines is clearly showing here, but im wondering do you mean as a class entirely they are considered alks or just certain ones are?
 
 
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