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What is wrong with the MDMA available today? - v2

ThreePointCircle said:
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.
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If you go for a larger ammounts like 10-40g then yes

Otherwise it would be good to seperate and TLC spot plate test as well
 
user666 said:
At any pH ?
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No when you titrate up or down it's very pH specific

You can actually relock your MDMA using too much base making it back to free base. Some call it a lock out you would need to add more HCL again to unlock it

Also when adding base kOH or NaOH or acids. First it's exothermic it will raise the temp of the solute especially if you go too fast. You should add a little at a time. Mix till dissolved, wait 3-5 min test ph again, repeat

Mixing it with water is **very exothermic**, which means it produces lots of heat.

If your water is warm to begin with and you add too much lye at once, the heat produced as it dissolves can easily bring the solution to the boil - which is obviously a very bad situation considering there aren’t many materials that aren’t easily destroyed by hot concentrated lye (namely your skin, eyes/vision, glass). It will violently boil and splash hot lye everywhere.

You want to make sure that add it very slowly and carefully - let the mixture cool down in between additions. Make sure you are adding the lye to the water and not the other way round - having lots of water will help dissipate the heat.

You want to be wearing gloves, safety goggles and a labcoat at all times. If you get any contamination on your gloves then they need to be removed straight away.

You want to have quick access to a shower / sink where you can wash yourself should you spill any chemicals over yourself.

It’s best to have someone with you while you work.

https://www.coleparmer.com/chemical-resistance chemical comparability charts will help you select appropriate materials. There are also charts to check that relate specifically to gloves.

Here is the safety data sheet: https://www.sigmaaldrich.com/MSDS/r...B&language=EN&productNumber=S0899&brand=SIGMA

Just a cautionary tale;

I was making biodiesel for school once. Added a few grams of Naoh, few hundred mils of methanol to a quart of vegetable oil. It almost melted the apple juice container, and the pressure generated almost made it explode bc the cap was on. Live and learn.

Maybe duh, but: look into soap making tutorials where people use lye. They'll have lots of useful tips. Also, ya, very very exothermic. We always cooled our water/isopropanol solutions in an ice bath before dissolving hydroxides in them, and they'd still heat up a ton.

Most importantly: wash it off your skin IMMEDIATELY if you get it on you, even little splashes. In my experience, it burns much "worse" than even strong acid.



When it comes to gasing just get HCL gas already predisolved in methanol or ISOPROPYL alcohol in 5/6 N OR M predisolved. This way no need to gas. Just titrate

Might be a little harder to find but much safer and easier then gassing and not impossible to find either

Also follow AAA. This applies to bases as well

ALWAYS ADD ACID.

ALWAYS ADD base or acid to the solution

Don't add solution especially base to water.

Unless you want to show your class a cool volcano project without the need for baking soda/vinegar
 
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ThreePointCircle said:
Very interesting. The frustration that has existed since the first page of the first thread is that analysis could answer the question, but the services available to the public tend to just say 'pure as the driven snow' while forensic papers always talk about contaminants relating to the synthesis procedures. I remember one of the authors of the MDDMA inhibitor paper was asked how much it would take to have the 'meh' effect, and while they didn't know, they speculated that it could be a small amount. So anything else in the sample could be relevant but goes unreported by the testing services.
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Yes happens a lot sadly
 
ThreePointCircle said:
I've chased up Kykeon and the person I spoke to is chasing up their lab manager. Still been a couple of days though.

@vash445 when you do your double recrystallisation you're doing the 'slow cooling' method from https://chemistry.mit.edu/facilitie...iffraction-facility/growing-quality-crystals/ ?
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The last batches have been slow cooling that's what people have been enjoying.

I've been experimenting with a slow evap method as well when it comes to extremely dirty mother liquor product

Diffraction quality crystals need to be relatively large. Maybe not quite on the engagement ring scale, but 0.1 to 0.3 mm in each dimension is a good number. In order to grow large crystals, it is important to avoid having too many nucleation sites (see above). Crystals that grow more slowly, tend to be larger. Mostly for crystals grown by slow cooling of the solvent: it sometimes improves the quality and size of the crystals if the solution is slowly warmed up until almost all crystals are dissolved again and then cooled down a second time very slowly. This can reduce the number of crystals obtained and usually improves quality and size.

No need to bring the beaker to the hotplate . This can simply be done heating up the room with a space heater, the HVAC thermostat or even running a dehumidifier in the room and there by increasing the temperature of the room. It is always a good idea to not change the environmental conditions for your crystals too often. When possible, leave them alone.



I've done all 3 method of recrystallization typically outlined here/ mitcjust depends how I feel experiment wise with the lab coat and hat sorta deal. Slow evap , slow temp, co solvent

I wasted time, now time doth waste me
A good crystal grows slowly. A good time frame for a crystallization experiment seems to be some two to seven days. Crystals that grow within minutes usually don’t diffract as well as they could

I was gonna say 3 days to 2 weeks depending what I'm going for crystal wise and how long it takes to grow

2 weeks might be a little long but if I'm in vacation or something it's whatever that's what double recrystallization is for anyways
 
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vash445 said:
The last batches have been slow cooling that's what people have been enjoying.

I've been experimenting with a slow evap method as well when it comes to extremely dirty mother liquor product

Diffraction quality crystals need to be relatively large. Maybe not quite on the engagement ring scale, but 0.1 to 0.3 mm in each dimension is a good number. In order to grow large crystals, it is important to avoid having too many nucleation sites (see above). Crystals that grow more slowly, tend to be larger. Mostly for crystals grown by slow cooling of the solvent: it sometimes improves the quality and size of the crystals if the solution is slowly warmed up until almost all crystals are dissolved again and then cooled down a second time very slowly. This can reduce the number of crystals obtained and usually improves quality and size.

No need to bring the beaker to the hotplate . This can simply be done heating up the room with a space heater, the HVAC thermostat or even running a dehumidifier in the room and there by increasing the temperature of the room. It is always a good idea to not change the environmental conditions for your crystals too often. When possible, leave them alone.



I've done all 3 method of recrystallization typically outlined here/ mitcjust depends how I feel experiment wise with the lab coat and hat sorta deal. Slow evap , slow temp, co solvent

I wasted time, now time doth waste me
A good crystal grows slowly. A good time frame for a crystallization experiment seems to be some two to seven days. Crystals that grow within minutes usually don’t diffract as well as they could

I was gonna say 3 days to 2 weeks depending what I'm going for crystal wise and how long it takes to grow

2 weeks might be a little long but if I'm in vacation or something it's whatever that's what double recrystallization is for anyways
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It's been a while since I tried recrystallisation and I'm not a chemist so I've forgotten most of what I know. Looking at some videos and other resources I'm getting my head back in the game but a couple of questions:

1) Should I do just acetone, or the isopropyl + acetone method suggested by @unodelacosa ? I'm happy with either as long as I konw what I'm doing
2) If just acetone, do you bring that to the boil before adding to the mdma or a set temp?
3) For these long cool downs, can you just leave on the hotplate and gradually reduce the temp setting over time?
4) One video I saw used a water both beaker with two test tubes suspended. One with the substance, and one with the solvent. Is this a good setup or do I just heat up solvent, pipette to separate beaker with mdma until dissolved, and then move the disolved mdma onto the hotplate for the long cool down procedure?
5) When cooling down, should I cover/seal beaker/tube with aluminium foil
6) Should I insert a hot filtration step? That seems quite common

I'm not concerned with yield, only quality to maximise chances of it working.

Thanks
 
ThreePointCircle said:
It's been a while since I tried recrystallisation and I'm not a chemist so I've forgotten most of what I know. Looking at some videos and other resources I'm getting my head back in the game but a couple of questions:

1) Should I do just acetone, or the isopropyl + acetone method suggested by @unodelacosa ? I'm happy with either as long as I konw what I'm doing
2) If just acetone, do you bring that to the boil before adding to the mdma or a set temp?
3) For these long cool downs, can you just leave on the hotplate and gradually reduce the temp setting over time?
4) One video I saw used a water both beaker with two test tubes suspended. One with the substance, and one with the solvent. Is this a good setup or do I just heat up solvent, pipette to separate beaker with mdma until dissolved, and then move the disolved mdma onto the hotplate for the long cool down procedure?
5) When cooling down, should I cover/seal beaker/tube with aluminium foil
6) Should I insert a hot filtration step? That seems quite common

I'm not concerned with yield, only quality to maximise chances of it working.

Thanks
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I used just acetone it's just hard to dissolve product you can do a mix of both to help dissolve. Crash out etc. The key is go slow crystals should take a week approx... And be 1 -3 mm / kcrat. For a two-solvent recrystallization, you should have one solvent (solvent #1) in which your desired compound is soluble at the boiling point. The second solvent (solvent #2) should induce crystallization when added to a saturated solution of your compound in the primary solvent. Typically this can crash out crystals faster. Personally I like to wait as I like less neculation sites.I've often found the precipitation done wrong leads to such a fine powder that you have to use a fine frit, which either takes forever or immediately gets clogged and stops working. Urgh.

Isolating by centrifuge can work but doesn't scale and can be painful.

2. You can do either or just make sure it all disloves you typically want it slightly under the boiling point of solvent or melting point of the MDMA. It will take a bit to dissolve with just acetone

3. You will filter it so you can transfer to another beaker that's sitting in hot water and gradually change said hot water over time

4. That sounds like Convection
Albeit somewhat exotic, convection can be a good method to grow high quality crystals. the other recrystallization technique described in the MIT LINK. Is that what you are talking about?

5. You can it will help slow the cool down

6. There's a lot of junk usually hair nail etc so yes
 
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Thanks. No it wasn't convection. Just a way of setting things up but my bad explanation made it sound more interesting. Doesn't really matter, what you have explained makes sense.

So basically if you crystallise too fast you get the impurities locked in the crystal?
 
Another thing that went downhill is the ket. I noticed it myself and other people have commented. It has a jittery kind of feeling to it. Some theorise that it could be the MSG it's often cut with, but you can taste it when it's in there and I've not noticed it in any of the batches, the meaty taste.
 
Well I've started the recrystallisation. Just went for straight acetone with 1g of "mdma". The method I went for in the end, was to have the mdma + acetone beaker on the hotplate and slowly in stages added more acetone and let it come to a soft boil, until the crystal disappeared. Took a while and quite a bit of acetone (read about 55ml in the flask for 1g of mdma) but worked. I put it into a filter into another beaker which is currently sitting in a water bath in yet another beaker, sitting on the hotplate, holding at a steady dissolved state.

I plan to slowly lower the temp of the hotplate and see what happens.
 
Hmm, something wrong in my procedure. I have the mdma dissolved in acetone in a small beaker covered by aluminium. That is in a water bath also covered in aluminium. That is on a hotplate. I left it in a non-boiling state and had a look at it this morning. Quite a bit of the acetone has evaporated even in that setup and crystals are forming.

Should I have set it to a colder level? Was concerned about it crashing out too fast due to too low a temp but it seems to be crashing out too fast due to evaporation.
 
ThreePointCircle said:
Hmm, something wrong in my procedure. I have the mdma dissolved in acetone in a small beaker covered by aluminium. That is in a water bath also covered in aluminium. That is on a hotplate. I left it in a non-boiling state and had a look at it this morning. Quite a bit of the acetone has evaporated even in that setup and crystals are forming.

Should I have set it to a colder level? Was concerned about it crashing out too fast due to too low a temp but it seems to be crashing out too fast due to evaporation.
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If it crashes out to fast you can reheat to disloves the crystals


Next question was the beaker you filtered INTO HOT?

THE BEAKER on the hot water bath you need to filter into needs to be HOT

some put it in the oven

I just make sure I have boiling hot water and have that beaker sit in hot water till it is HOT

also

When once that is hot and you have filtered INTO into make sure that water is hot and you consistently replace the hot water I have no problems with evaporated acetone

If you are you are either going to hot

Or your saturated solution isn't saturated ENOUGH

It should BE VERY HARD to dissolve larger ammounts of MDMA into acetone

What temps are you using?

And ammounts of MDMA are you using?

Crystals should take 2 days to form


Ohhhh wait a second I think I know your problem I bet you are using a WIDE MOUTH BEAKER?

Switch to a narrow end flat bottom beaker that is typically of boiling flask

It can be a flat bottom round boiling flask. Erlenmeyer flask with screw closure, or a conicol

Or it can be round if on a mantel just make sure it's a boiling flask DURNING the heating process.

You may also need to raise the temperature a bit so it cools down slower
 
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This no



The greater the surface area the quicker the EVAP rate

If you are using a beaker like this after you filter evaporated acetone will happen much faster than a distilling flask
 
ThreePointCircle said:
Hmm, something wrong in my procedure. I have the mdma dissolved in acetone in a small beaker covered by aluminium. That is in a water bath also covered in aluminium. That is on a hotplate. I left it in a non-boiling state and had a look at it this morning. Quite a bit of the acetone has evaporated even in that setup and crystals are forming.

Should I have set it to a colder level? Was concerned about it crashing out too fast due to too low a temp but it seems to be crashing out too fast due to evaporation.
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See comments above to fix issues
 
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