What is wrong with the MDMA available today? - v2

[ThreePointCircle]

Did you ask for an inpurity report vs a what is this report?

A seperation with chromotrographyand analysis is the waay to go maybe with added HPLC that will you get the report you are looking for.

also maps grain size is .1 to .3 ckar

I went for their most expensive report which was the quantative option, and also asked them about all those query substances.

More than that I don't know. All I have is that report I linked.

I don't know where to send it to get a better analysis.

 

[vash445]

I went for their most expensive report which was the quantative option, and also asked them about all those query substances.

More than that I don't know. All I have is that report I linked.

I don't know where to send it to get a better analysis.

No you went for their most common

You need a CUSTOM REQUEST TO SEPERATE THE 8% AND TEST ONLY SPECIFICALLY THAT with HPLC and NMR

Can you perform custom analyses?
Yes! We are happy to perform a custom analysis for your sample. If you would like us to do a custom analysis for your sample, for instance doing a specific NMR or mass spectrometry experiment, or if you want us to follow a specific extraction procedure or quantify a specific minor alkaloid in a plant, then please don’t hesitate to contact us with your request. We always strive to find solutions for each user’s specific needs and we are always happy to expand the analyses that we offer.

 

[ThreePointCircle]

No you went for their most common

You need a CUSTOM REQUEST TO SEPERATE THE 8% AND TEST ONLY SPECIFICALLY THAT with HPLC and NMR

Can you perform custom analyses?
Yes! We are happy to perform a custom analysis for your sample. If you would like us to do a custom analysis for your sample, for instance doing a specific NMR or mass spectrometry experiment, or if you want us to follow a specific extraction procedure or quantify a specific minor alkaloid in a plant, then please don’t hesitate to contact us with your request. We always strive to find solutions for each user’s specific needs and we are always happy to expand the analyses that we offer.

Ok, a few things.

I approached them and specifically asked for an analysis to find impurities. I listed the items of interest that others suggested on here, but in the framework of what we were talking about here, and asked if they could do them and which option they suggested. They said they could and said select the full quantitative + qualitative option. That was €90 which is the top of the line option (albeit not expressed as a custom option).

If this is a communication issue then maybe it's worth another go with them but I'm not too impressed they didn't recommend the right path. I see what you've listed is from the FAQ but do we have any confirmation that they are capable from a resource and skills point of view to do what you suggest?

If so I'll contact them again. But if I do, can I have the exact wording of what to ask for so there's no ambiguity?

 

[ThreePointCircle]

Since you gave me a thumbs up for the inadvertent Fentanyl cross-contamination, I'll reciprocate with a procedure to separate MDMA from Fentanyl and its analogs by exploiting their different pKA in AB extractions:

• Dissolve: 1g sample of contaminated MDMA·HCl in 20mL warm distilled water.
• Filter (e.g.coffee filter) → clear solution.
• Basify: Slowly dilute with 1M solution of NaOH dropwise to pH 9.2-9.5 (use precise pH meter). Don't overshoot!
• Extract: Add 50mL Xylene, shake 10min, wait for layers to separate (fentanyls go into the top organic layer - discard it).
• Repeat: Repeat the former extraction 5x, maintain pH 9.2-9.5, discard all organic layers, keep the aqueous layers (do not reuse the same glassware).
• Acidify: Dilute with HCl to pH 6 → MDMA·HCl crashes out.
• Evap/Filter: Recrystallize from hot IPA/acetone (slowly cool → white crystals).
  
  Note: Toluene or Naphtha can be used in lieu of the Xylene.

I invite the more experienced chemists here to refine this procedure.

Just checking, this isn't the OH group selective acid-base liquid-liquid extraction is it? It's just for Fentanyl removal?

 

[vash445]

Ok, a few things.

I approached them and specifically asked for an analysis to find impurities. I listed the items of interest that others suggested on here, but in the framework of what we were talking about here, and asked if they could do them and which option they suggested. They said they could and said select the full quantitative + qualitative option. That was €90 which is the top of the line option (albeit not expressed as a custom option).

If this is a communication issue then maybe it's worth another go with them but I'm not too impressed they didn't recommend the right path. I see what you've listed is from the FAQ but do we have any confirmation that they are capable from a resource and skills point of view to do what you suggest?

If so I'll contact them again. But if I do, can I have the exact wording of what to ask for so there's no ambiguity?

Hi, to Rafael at your company I recently used your services and was unimpressed, I hope this may clear up any ambiguity and we can reuse your service moving forward again. I believe my last inquiry may have left ambiguity in my current academic research into this matter for my college dissertation in the effects of different impurities effecting inhibitors block sert H2T BLAH BLAH. One of many associates who recommended you may have found the miscommunication breakdown between us. I work in law/enforcement/civil services drug treatment humanity/anthropology and I don't understand chemistry or analytics


Maybe I requested the wrong thing.. I'm not interested in the main component. I'm interested in finding out the side products

If I test again. I need to know the 8 not the 92%

Can you perform a column chromotography or similar like an acid base to seperate the known MDMA from the unknown 8% with the lab file on hand and provide the optimal lab work for seperation and why it was chosen with the lab sample and tests as provided for and done before or after.

Please run an NMR, HPLC or paper spray mass spec to finger print the 8% impurities alone by it self. Please preform a MALDI or similar test to figure out of the mol weight is different then MDMA If your graphs don't tell you the best values for optimal column chromotography, please feel free to do a comprehensive spot check on TLC to help. Please provide what the method to remove the 8% was chosen and why you set up the column to target said micro impurities. I'm also interested in any potential residual solvents and if it's hydrated or unhydrate form of MDMA.



I have no need to know my MDMA is X% purity. We already know it is of 90% consistently so that does not concern my current academic research and the university of bluelight currently college resident of E-stone INA

I need to know what other impurities are in MDMA is in currently with my MDMA with lab point precision and hopefully includes any potential residual solvents, hydrates polymorphs etc

I hope this may clear up any misunderstanding we may have. I hope my report may look like this example above

Please ignore any major MDMA or peaks. Unless stuff like MDMMA /ETC Please provide a clear picture of any impurities and if possible a MALDI or similar to find molecular weight on the 8% impurities

Not on the substance as a whole

My objective is to paint a clear picture to find out which impurities are in this sample and the values you used for chromotography and why they were chosen before running the sample to fingerprint solely on impurities.

My academic research hinges on knowing the major lab non pharma impurities on street drugs effects on the human bodies and its potential to block effective bioavailability of drugs to produce effects my target is solely impurities identification into great detail similar to the example provided above...

I please ask whether they are capable of doing some sensitive tests for the presence of low-concentration OH groups or other low-concentration impurities. The trifecta would be an XRF or similar to see what type of MDMA it is. Form 1 form 2, form 3 or form 4 if it exists. I understand this probably a custom request looking at your FAQ.

Did you get it as the typical giant block and they what I believe is called slow melt reforming or did it look different?

Sincerely,

3 point circle

Suggestions anyone?

 

[ThreePointCircle]

I'll give it a go and see what they say

 

[vash445]

I'll give it a go and see what they say

Please note I see BOTH side and do not blame you, I do not blame them. But they suggested the typical you go the typical I want everything in this sample but you didn't need that trst

You needed the custom request

You can also ask because of the miscommunication you understand this custom test might cost more but you are hoping you can get it partially waived with the cost of the previous test all things considered.

Couldn't hurt to ask to turn things around

But I don't blame either side so or what anyone suggested here. Some have better knowledge then others, some might not have known the full picture like you etc etc

I do NOT blame either party and now see this type of work maybe a custom request Etc etc

 

[vash445]

Just checking, this isn't the OH group selective acid-base liquid-liquid extraction is it? It's just for Fentanyl removal?

Acid base is for all impurities

Soap, making MDP2P from glaciated MDP2P. DMT etc etc uses acid base.


removal just like column chromotography, recrystallization convert to base and redistilling base then recrystallization if a column doesn't help

 

[ThreePointCircle]

I hope this may clear up any misunderstanding we may have. I hope my report may look like this example above

What example were you referring to? I'm just writing up my email to them.

Did you get it as the typical giant block and they what I believe is called slow melt reforming or did it look different?

I got it as crushed crystal. The usual market stuff.

 

[ThreePointCircle]

Ignore that last question, I've emailed them. Well report back...

 

[vash445]

Ignore that last question, I've emailed them. Well report back...

That other lab report you posted here thinking it would be like that?

 

[ThreePointCircle]

That other lab report you posted here thinking it would be like that?

Oh I see. No problem. I kind of said that in the email to them so all good

 

[vash445]

I went for their most expensive report which was the quantative option, and also asked them about all those query substances.

More than that I don't know. All I have is that report I linked.

I don't know where to send it to get a better analysis.

Well yes neither do I but I don't think they knew what you truly wanted. This is a more ummm custom request

Then what THEY THINK the avg consumer wants for get for $90

Who runs NMR for $90 euro? Noone

Who provides papers and someone pointed out an OH contam peak? Almost noone except energy control and I've posted my issues with them

Reading the results is half the battle in this so to speak. You got what you paid for what they assumed you wanted which is fair. There are steps AFTER that I outlined above

My college is like $150 or $200 hr unassisted to run a Burker NMR but anyone can use it assisted is $350 hr

 

[vash445]

Oh I see. No problem. I kind of said that in the email to them so all good

Also not everyone would catch that OH contam peak read these is HALF the battle

That's why alot of people ask to post and see if they see anything someone might miss

You got and paid for what they assumed you asked. It is fair reguardless what you got. See how much more expensive your new requests is

But you got for 90 is fair. Let's just take the next steps which is something on custom order any basic lab like this should be able to do an acid base or column chromotography upon special requests

I'm saying no one was wrong. I think just both parties didn't explain what you are getting vs what you really want sorta deal. There was a lack of I analytics nerd speak to step in to explain like I'm 5

 

[ThreePointCircle]

I hear what you're saying although as a public testing facility I would assume they are subsidised to some extent. I don't think my original request could be interpreted as asking for just the identification of the main component. In fact, I clearly said contaminants/by-products - which they said they can do. If they couldn't, or couldn't for the price, then they should have said. Tbh, I'm not really seeing what they did was any more than Wedinos would have done for free.

Anyway, water under the bridge, let's see how they respond now.

 

[unodelacosa]

Since you gave me a thumbs up for the inadvertent Fentanyl cross-contamination, I'll reciprocate with a procedure to separate MDMA from Fentanyl and its analogs by exploiting their different pKA in AB extractions:

Not recommended; please see my notes.

• Dissolve: 1g sample of contaminated MDMA·HCl in 20mL warm distilled water.
• Filter (e.g.coffee filter) → clear solution.
• Basify: Slowly dilute with 1M solution of NaOH dropwise to pH 9.2-9.5 (use precise pH meter). Don't overshoot!

NOTE: The Na from the NaOH will combine with the Cl from the HCl, and it will form NaCl, aka: table salt. The remaining two hydrogens and oxygen combine to form H₂O. So salt water is a side product here, but this frees up the MDMA base (thus making it "freebase", you see), and it will do this to all other compounds in the solution that also have an amine group (NH₃). These will then move into the non-polar solvent layer (Xylene or whatever).

• Extract: Add 50mL Xylene, shake 10min, wait for layers to separate (fentanyls go into the top organic layer - discard it).

NOTE: You will be discarding MDMA freebase oil in the top/Xyelene layer. Do not do this.

• Repeat: Repeat the former extraction 5x, maintain pH 9.2-9.5, discard all organic layers, keep the aqueous layers (do not reuse the same glassware).

Do not do this. This would discard all the active ingredients while keeping salt water behind.

• Acidify: Dilute with HCl to pH 6 → MDMA·HCl crashes out.

Nothing would crash out. If there were any MDMA left it would bond to the acid and become water soluble instantly, and it would be dissolved in the water. Instead, you've discarded it, and the only thing that will be left behind is some salty-ass water.

• Evap/Filter: Recrystallize from hot IPA/acetone (slowly cool → white crystals).

This part is closer to being correct, but again, you will have tossed out your product.

• Note: Toluene or Naphtha can be used in lieu of the Xylene.

I invite the more experienced chemists here to refine this procedure.

Naphtha isn't a great substitute for Xylene. It has to at least be heated first before using it.

There's no kitchen chemistry procedure for removing fentanyl from MDMA if that were to have happened. If you're using fent test strips be aware that they give false positives occasionally. Test things several times if you're really concerned.

Regardless, the right way to do this procedure is when you raise the pH over 7 (neutral), the water will become basic instead of acidic or neutral. At that point, you will be keeping the non-polar layer. You extract from the aqueous layer two more times, each time keeping the NP layer. Then you combine them and discard the water layer. Next you want to wash the NP solution, so you add a bit of water (maybe like ¼ of the solution volume), shake it, let separate and discard the water layer. Do it once more with some salt water (helps "scrub" the NP layer clean, so to speak), and again discard the water layer.

Next you need to dry the NP solution by running it through some dry MgSO₄ (bake epsom salts in the oven for 30 min at 300° or whatever until it's dusty dry and presto! magnesium sulfate). Then you gas it with anhydrous HCl gas (there are procedures for this on the erowid's archive of Rhodium.ws). Crystals in tow, proceed to recrystallizing them slowly from a two-solvent matrix of first boiling IPA to the point of saturation, and then secondly ice-cold anhydrous acetone. Do this extra slowly and you will be blessed with aesthetically pleasing crystals of very clean MDMA, assuming no other amine-bearing compounds are present.

Otherwise you'd need to get into chromatography columns and/or vacuum distillations…

 

[ThreePointCircle]

NOTE: You will be discarding MDMA freebase oil in the top/Xyelene layer. Do not do this.

I looked at the old procedure I did and it said the same as you - the freebase is in the xylene layer. I think I had a pretty good go at the procedure when I did it. The recrystallisation could have been a bit sloppy. That aside, I don't know if giving the procedure another go would be worthwhile?

But maybe I should have another go at the recrystallisation as @vash445 suggests.

There's no kitchen chemistry procedure for removing fentanyl from MDMA if that were to have happened. If you're using fent test strips be aware that they give false positives occasionally. Test things several times if you're really concerned.

The test came back as negative. It gives a line for a negative result - absent for positive so it felt like a positive negative result if that makes sense.

Otherwise you'd need to get into chromatography columns and/or vacuum distillations…

Back in the day I had a bit of a go at vacuum distillation but didn't get very far. I'm trying to remember what the issue was. Maybe it was the volumes of product were too small and I was struggling to get the process going properly. I would be happy to give it another go but maybe I need to understand what is needed if you're only dealing with a gramme or two of product.

I assume chomatogarphy columns is a non-starter for kitchen chemistry?

 

[vash445]

I looked at the old procedure I did and it said the same as you - the freebase is in the xylene layer. I think I had a pretty good go at the procedure when I did it. The recrystallisation could have been a bit sloppy. That aside, I don't know if giving the procedure another go would be worthwhile?

But maybe I should have another go at the recrystallisation as @vash445 suggests.


The test came back as negative. It gives a line for a negative result - absent for positive so it felt like a positive negative result if that makes sense.


Back in the day I had a bit of a go at vacuum distillation but didn't get very far. I'm trying to remember what the issue was. Maybe it was the volumes of product were too small and I was struggling to get the process going properly. I would be happy to give it another go but maybe I need to understand what is needed if you're only dealing with a gramme or two of product.

I assume chomatogarphy columns is a non-starter for kitchen chemistry?

Even more so diy and cheaper then a vac distilled at home

Just slow when working with large amounts unless you got a 4story column XD

 

[vash445]

I looked at the old procedure I did and it said the same as you - the freebase is in the xylene layer. I think I had a pretty good go at the procedure when I did it. The recrystallisation could have been a bit sloppy. That aside, I don't know if giving the procedure another go would be worthwhile?

But maybe I should have another go at the recrystallisation as @vash445 suggests.


The test came back as negative. It gives a line for a negative result - absent for positive so it felt like a positive negative result if that makes sense.


Back in the day I had a bit of a go at vacuum distillation but didn't get very far. I'm trying to remember what the issue was. Maybe it was the volumes of product were too small and I was struggling to get the process going properly. I would be happy to give it another go but maybe I need to understand what is needed if you're only dealing with a gramme or two of product.

I assume chomatogarphy columns is a non-starter for kitchen chemistry?

You can create a simple chromatography column at home using a syringe, cotton, sand, and water or rubbing alcohol, similar to the method described in a guide from the North Carolina Museum of Natural Sciences. First, prepare the column by placing a cotton ball in the bottom of the syringe, followed by layers of sand. Then, add your liquid sample and allow the mobile phase (like water or alcohol) to separate the mixture as it travels through the column and drips out, where you can collect the different components.

Filter media for column chromatography includes silica gel 60 for standard separations, regenerated cellulose or other compatible membranes for protein purification, and various specialized resins like anion exchange media for specific molecular target

1. Choice of Silica or Alumina for the Stationary Phase
Silica and alumina are both polar adsorbents so the more polar components in the mixture to be separated are retained more strongly on the stationary phase and are therefore eluted from the column last. Silica is recommended for most compounds, but as it is slightly acidic, it preferentially retains basic compounds. Alumina is slightly basic, so will retain acidic compounds more strongly. It is good for separation of components that are weakly or moderately polar and the purification of amines.

Absorbent particle size affects how solvent flows through the column. Silica or alumina are both available in a variety of sizes.

The size is given by the mesh value which refers to the number of holes in the mesh that is used to sieve the absorbent. Thus higher mesh values such as “silica gel 230–400” have more holes per unit area and correspondingly smaller particles than “silica gel 60”. Typically, 70–230 silica gel is used for gravity columns and 230–400 mesh for flash columns.

 

[ThreePointCircle]

You can create a simple chromatography column at home using a syringe, cotton, sand, and water or rubbing alcohol, similar to the method described in a guide from the North Carolina Museum of Natural Sciences. First, prepare the column by placing a cotton ball in the bottom of the syringe, followed by layers of sand. Then, add your liquid sample and allow the mobile phase (like water or alcohol) to separate the mixture as it travels through the column and drips out, where you can collect the different components.

Filter media for column chromatography includes silica gel 60 for standard separations, regenerated cellulose or other compatible membranes for protein purification, and various specialized resins like anion exchange media for specific molecular target

1. Choice of Silica or Alumina for the Stationary Phase
Silica and alumina are both polar adsorbents so the more polar components in the mixture to be separated are retained more strongly on the stationary phase and are therefore eluted from the column last. Silica is recommended for most compounds, but as it is slightly acidic, it preferentially retains basic compounds. Alumina is slightly basic, so will retain acidic compounds more strongly. It is good for separation of components that are weakly or moderately polar and the purification of amines.

Absorbent particle size affects how solvent flows through the column. Silica or alumina are both available in a variety of sizes.

The size is given by the mesh value which refers to the number of holes in the mesh that is used to sieve the absorbent. Thus higher mesh values such as “silica gel 230–400” have more holes per unit area and correspondingly smaller particles than “silica gel 60”. Typically, 70–230 silica gel is used for gravity columns and 230–400 mesh for flash columns.

Do you know what, I think I did have a go at doing a column. It was so long ago I forgot. I didn't get any good results but do you think it would be worth having another go?

Maybe column + recrystallisation?

I think my idea back in the day was to collect a load of fractions and then test them with reagents to see which one(s) had the mdma in it but I made a bit of a mess of it and didn't have another go.