I had some relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, even the tests shown purity around 95. Crystallization of oversaturated water solution didn't bring any result, as well as acetone. So I decided to make an attempt with IPA as the last resort.
The report about result will come later. But I can say now, the volume of IPA mentioned by noble @G.Patton is quite excessive. I had 22 gr, so I started with 80 ml of IPA. Then, as it started boiling - 82.6C, I removed some volume down to 60 ml, and slowly added the salt. It dissolved completely without any difficulty. So I kept it on the hotplate for a while.
At the ending, as I was able to see powder rising in the beaker (but it could be some insoluble impurities as well) total volume was 71 ml. The salt itself shall take 22.0/ 1.1 = 20 ml. So IPA volume shall be 71 - 20 = 51 ml, that means 1 ml of hot boiling IPA solves at least 0.43 gr of MDMA HCl or even more, let's see.
IPA purity is >99.5.
Might be, it is better to start with 20 ml of IP per 10 gr of MDMA?
The report about result will come later. But I can say now, the volume of IPA mentioned by noble @G.Patton is quite excessive. I had 22 gr, so I started with 80 ml of IPA. Then, as it started boiling - 82.6C, I removed some volume down to 60 ml, and slowly added the salt. It dissolved completely without any difficulty. So I kept it on the hotplate for a while.
At the ending, as I was able to see powder rising in the beaker (but it could be some insoluble impurities as well) total volume was 71 ml. The salt itself shall take 22.0/ 1.1 = 20 ml. So IPA volume shall be 71 - 20 = 51 ml, that means 1 ml of hot boiling IPA solves at least 0.43 gr of MDMA HCl or even more, let's see.
IPA purity is >99.5.
Might be, it is better to start with 20 ml of IP per 10 gr of MDMA?
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↑View previous replies…
- By Mr Good Cat
probably my hands are growing out of my ass. i did as i described above, coolled the beaker down to RT, and put it in the freezer for 2 hours. then, all I see, the whole RM is completely frozen piece of ice. is there any suggestion what to do? repeat the procedure with additional IPA in the RM?
↑View previous replies…
- By Mr Good Cat
It is not about color. The problem is all the RM (MDMA HCL + IPA) turned to the piece of ice (or rather a kind of dense porridge).
I even added 20 ml of IPA to increase total RM to 80 ml, and left it not in the fridge instead of freezer for a while with the same result: total RM turned into the same porridge without any chance to saperate dirty IPA from chloride.
I even added 20 ml of IPA to increase total RM to 80 ml, and left it not in the fridge instead of freezer for a while with the same result: total RM turned into the same porridge without any chance to saperate dirty IPA from chloride.
- By Mr Good Cat
yes, I have a feeling that the salt precipitates too quickly. may be, it could be right to leave the beaker on RT for 5-8 hour to see what is going on.
Four attempts of IPA crystallization. Fulll report with quantities, volumes and timing
or FAST IS ALWAYS BAD!
IPA purity is >99.5.
Relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, apart of the fact the tests shown purity around 95. Weight of sample - 22 gr, calculated volume of sample - 22 / 1.1 = 20 ml.
Stirring hotplate used.
All the coolings are done with the beaker hermetically closed to avoid moisture from the air catching.
1. First I prepared 60 ml of boiling IPA 82.6C on the stirring hotplate, then put the salt, that dissolved immediately. Considering such fast dissolvation, I decided, the volume of IPA was too huge and evaporated some.
The beaker was left on the hotplate to cool down to RT, that took 80 minutes approx., then moved it to the freezer.
The result came after one hour as a dense porridge without any trace of dirty IPA.
Total volume of RM after warming up to RT was 62-63 ml, that means the remains of IPA was 42-43 ml.
Result: FAULT!
2. RM was warmed up to RT, then certain IPA was added with some stirring to increase the volume of RM up to 87 ml under RT.
RM was heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the freezer.
The result was checked after 5-6 hours: dense porridge again.
Result: FAULT!
3. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the fridge.
The result was checked after 1 hours: dense porridge again.
Result: FAULT!
4. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, and left at RT for a while. As 120 minutes gone after heating was finished: some crystalls appeared at the bottom. Total volume of RM at this point was 81 ml - that means around 6 ml was evaporated while heating up.
Then I left RM at RT for 240 minutes more. As 240 minutes gone, the crystalls became pretty visible and transparent.
So, the beaker was moved to the fringe for 2 hours without any noticable changes.
With the next step the beaker was moved to the freezer to finish the process.
Result: SUCESS!
Hope, this full description will help some newbies with volume and timing estimation and let them avoid my mistakes.
Total yeld is 18.5 gr.
3.5 gr are somewhere in the dirty IPA or evaporated(((
or FAST IS ALWAYS BAD!
IPA purity is >99.5.
Relatively small amount of MDMA HCl made from the freebase left for the overnight in the beaker. So the color was obviously slighty brownish or yellowish, whatever, but far away from the desirable color, apart of the fact the tests shown purity around 95. Weight of sample - 22 gr, calculated volume of sample - 22 / 1.1 = 20 ml.
Stirring hotplate used.
All the coolings are done with the beaker hermetically closed to avoid moisture from the air catching.
1. First I prepared 60 ml of boiling IPA 82.6C on the stirring hotplate, then put the salt, that dissolved immediately. Considering such fast dissolvation, I decided, the volume of IPA was too huge and evaporated some.
The beaker was left on the hotplate to cool down to RT, that took 80 minutes approx., then moved it to the freezer.
The result came after one hour as a dense porridge without any trace of dirty IPA.
Total volume of RM after warming up to RT was 62-63 ml, that means the remains of IPA was 42-43 ml.
Result: FAULT!
2. RM was warmed up to RT, then certain IPA was added with some stirring to increase the volume of RM up to 87 ml under RT.
RM was heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the freezer.
The result was checked after 5-6 hours: dense porridge again.
Result: FAULT!
3. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, then moved to the fridge.
The result was checked after 1 hours: dense porridge again.
Result: FAULT!
4. RM was warmed up to RT with some stirring, then heated up to 75 C till total dissolving. Then colled down to RT at the hot plate (same as before), that took 80 minutes, and left at RT for a while. As 120 minutes gone after heating was finished: some crystalls appeared at the bottom. Total volume of RM at this point was 81 ml - that means around 6 ml was evaporated while heating up.
Then I left RM at RT for 240 minutes more. As 240 minutes gone, the crystalls became pretty visible and transparent.
So, the beaker was moved to the fringe for 2 hours without any noticable changes.
With the next step the beaker was moved to the freezer to finish the process.
Result: SUCESS!
Hope, this full description will help some newbies with volume and timing estimation and let them avoid my mistakes.
Total yeld is 18.5 gr.
3.5 gr are somewhere in the dirty IPA or evaporated(((
- By G.Patton
Actually, it is acceptable color for mdma =)
I wrote in the topic Recrystallization and Hot Fltration (Lab FAQ section) that the slowest cooling have to be applied. Also, don't use freezer with -17*C. It is worth to cool down at 3-4*C in regular cooling camera of fridge.
You can evaporate IPA in mother liquor on a hot plate for about 1/2 or more and slowly cool it down to get second batch of a little bit dirtier crystals.
Anyway, congratulation and thank you for your full report with "FAULT!" results. It helps people to do not repeat same mistakes.
I wrote in the topic Recrystallization and Hot Fltration (Lab FAQ section) that the slowest cooling have to be applied. Also, don't use freezer with -17*C. It is worth to cool down at 3-4*C in regular cooling camera of fridge.
You can evaporate IPA in mother liquor on a hot plate for about 1/2 or more and slowly cool it down to get second batch of a little bit dirtier crystals.
Anyway, congratulation and thank you for your full report with "FAULT!" results. It helps people to do not repeat same mistakes.
- By Mr Good Cat
Yes, it is acceptable. The test with methanol and ruler also shows high percentage. Any way, we are looking for the purest product. This is why all these efforts.
I did it like this a long time ago:
1 Liter of Ipa (isopropyl alcohol) 99% laboratory grade (the "drugstore" grade does not work)
1 Liter of 99% acetone ("drugstore" grade does not work and less than Mercadona)
1 glass of 1 liter
1 hot plate (but since not everyone has it, a double boiler is an option)
1 laboratory thermometer
That's all.
For each gram of Mdma we need 3.50 ml of ipa (measurements are very important!)
We put the ipa in a beaker and also a thermometer touching the ipa
We heat the ipa to 55 degrees (do not exceed 60 degrees)
Once we have that temperature, we put the Mdma and it will dissolve
Cover the glass with a piece of paper and leave it at room temperature for 4 hours.
After those 4 hours it should be in the fridge for a day
the day after freezing for another day and the crystals are already forming
First batch:
Pour the dirty ipa into another glass and put it back in the freezer.
in the beaker with the crystals we add acetone (half ipa) the beaker is so cold that the crystals dissolve and the acetone blocks it.
approximately in an hour that same acetone we overturned it in the dirty ipa glass
We let the crystals dry for a day.
Why do we add acetone to the ipa? Because there are still crystals, but we need acetone, otherwise the crystals will not form.
With the discarded acetone we add it to the dirty ipa glass from the freezer. Without the acetone, the second batch of crystals won't form!
these crystals will take longer to form, leave them in the freezer for a few days
We took out the glass and threw away the dirty ipa.
We add acetone so that the crystals do not dissolve. When the glass is at room temperature, we throw away the acetone and let the crystals dry
1 Liter of Ipa (isopropyl alcohol) 99% laboratory grade (the "drugstore" grade does not work)
1 Liter of 99% acetone ("drugstore" grade does not work and less than Mercadona)
1 glass of 1 liter
1 hot plate (but since not everyone has it, a double boiler is an option)
1 laboratory thermometer
That's all.
For each gram of Mdma we need 3.50 ml of ipa (measurements are very important!)
We put the ipa in a beaker and also a thermometer touching the ipa
We heat the ipa to 55 degrees (do not exceed 60 degrees)
Once we have that temperature, we put the Mdma and it will dissolve
Cover the glass with a piece of paper and leave it at room temperature for 4 hours.
After those 4 hours it should be in the fridge for a day
the day after freezing for another day and the crystals are already forming
First batch:
Pour the dirty ipa into another glass and put it back in the freezer.
in the beaker with the crystals we add acetone (half ipa) the beaker is so cold that the crystals dissolve and the acetone blocks it.
approximately in an hour that same acetone we overturned it in the dirty ipa glass
We let the crystals dry for a day.
Why do we add acetone to the ipa? Because there are still crystals, but we need acetone, otherwise the crystals will not form.
With the discarded acetone we add it to the dirty ipa glass from the freezer. Without the acetone, the second batch of crystals won't form!
these crystals will take longer to form, leave them in the freezer for a few days
We took out the glass and threw away the dirty ipa.
We add acetone so that the crystals do not dissolve. When the glass is at room temperature, we throw away the acetone and let the crystals dry
Attachments
- By Mr Good Cat
As I understand, MDMA solubility in boiling IPA is around 1.4 ml of IPA per 1 gr of chloride.
May be, you can specify what is MDMA solubility in IPA at RT and frozen IPA?
May be, you can specify what is MDMA solubility in IPA at RT and frozen IPA?
- By Mr Good Cat
I empirically found interesting fact. Solubility in IPA depends on purity.
I had two batches, one after ABE, pure white, another one brownish after crystallization in water.
Both batches were solved by weight in IPA from the same bottle under T=65C.
Chloride weight - 70 gr
IPA weight - 193 gr
First flask dissolved completely.
Second flask got a problem with dissolvation: I had to add 9 gr of IPA to solve it completely. IPA weight was adjusted at the point of complete dissolvation in order to replenish the evaporated.
Also, as crystallization run, chloride flakes were seen floating on the surface in second flask. That wasn't noticed in first. Obviously density is different due to contaminants.
I had two batches, one after ABE, pure white, another one brownish after crystallization in water.
Both batches were solved by weight in IPA from the same bottle under T=65C.
Chloride weight - 70 gr
IPA weight - 193 gr
First flask dissolved completely.
Second flask got a problem with dissolvation: I had to add 9 gr of IPA to solve it completely. IPA weight was adjusted at the point of complete dissolvation in order to replenish the evaporated.
Also, as crystallization run, chloride flakes were seen floating on the surface in second flask. That wasn't noticed in first. Obviously density is different due to contaminants.
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Hi, i make a lot of purification of shity mdma, and now i have a problem.
I make the acetone washe, was nice i color not too bad.
Then disolve in hot IPA (very nice color clear) a crash crystals ,filter and dry.
Disolve again in IPA I want to make big crystals ( i do a lot of times) in hot satured IPA and seed the solution, this time i let the solution in the hot plate at 80 celcius all the night, the other day when i was going to start the slow ramp down temp for the grow... i see all The solution Dark! very nasty. i shut off the heat and let cool. Ends worse than when it started the really dirty shity sugared crystals. I let dry and make other acetone wash.. and have a looooot of oil when i evap the acetone from the second washes..! !
What the fuck is the redish dark oil? is soluble in water/alcohol/acetone
Maybe the heat can degrade MDMA hcl, or some impuritis?
PD: What you think about the antisolvent crash with acetone/ipa? when is better?
Can be a good one... free base the MDMA extract with diethyl ether and recrash with a few ml of chlorid acid 37%?
thanks boss
- By G.Patton
Hello, your MDMA reacted with oxygen in air. What a sense of heating at 80*C at night? I guess, all IPA was evaporated and your product was heated in a beaker at 80*C. You need to heat the solvent in order to increase MDMA solubility in the minimum amount of the solvent. Then, cool down it slowly in order to grow crystals.
Read more about Recrystallization and hot filtration
Read more about Recrystallization and hot filtration
↑View previous replies…
- By Macondor
The IPA was not evaporated because was in a seal flask with pressure, i do this a few times and grow big crystals, maybe it was lucky...?
So MDMA hcl react with oxigen and degrade to what? what is the oxidation product?
i think that MDMA was really heat resistent.
thanks
So MDMA hcl react with oxigen and degrade to what? what is the oxidation product?
i think that MDMA was really heat resistent.
thanks
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- By Macondor
After the acetone wash and one recrystallization in ipa can still be an excess of hcl? can you explain me more please?
There was a strong sweet aroma when i promt the second hot recrystallization when the red oil appeared, very strong. Now whats is left i wash with acetone like 6 times o 7 for clean again.. was a pain in the ass but.. lets see whats happen in a normal Recrystallization.
What do you think about an a/b metod for purification? Disolve in water Base with hidroxysodium and extract with diethyl ether and precipitate with hcl like shulgin in pikhal or bubble hcl gas.
thanks!!!
There was a strong sweet aroma when i promt the second hot recrystallization when the red oil appeared, very strong. Now whats is left i wash with acetone like 6 times o 7 for clean again.. was a pain in the ass but.. lets see whats happen in a normal Recrystallization.
What do you think about an a/b metod for purification? Disolve in water Base with hidroxysodium and extract with diethyl ether and precipitate with hcl like shulgin in pikhal or bubble hcl gas.
thanks!!!
- By G.Patton
No, there is no acid for sure. What a reason of your manipulations with boiling in IPA? I really don't understand your motivation. You are telling me that you've already washed your product and recrystallized. Doesn't your product testify you after this?
I posted the topic about a/b extraction of amphetamine. Here is same procedure with HCl gas instead of sulfuric acid.
I posted the topic about a/b extraction of amphetamine. Here is same procedure with HCl gas instead of sulfuric acid.
- By Macondor
I dont understand why dont crash white the crystals.. crash a litlle brown..and i make the second rex. i will do a 3 . Maybe is a reaction that start and can be stoped? When i heat the IPA for the second recrystallizations start to dark a litlle again
The method of adding drops of hcl 37% solution to the ether, will not work well? is more easy too me now,,
Is for grow big crystals..i do this a few times and work.. and with piperine to, at 70 celcius.. satured solution ,seeding cap the flask (are that ones for sterilzation and can hold pressure) and then slow down the temp in one or two days...only for fun i love see big crystals.
i do this a few times..and no problem.. maybe is something more in the product before the purification that react
thanks man sorry all questions..
The method of adding drops of hcl 37% solution to the ether, will not work well? is more easy too me now,,
Is for grow big crystals..i do this a few times and work.. and with piperine to, at 70 celcius.. satured solution ,seeding cap the flask (are that ones for sterilzation and can hold pressure) and then slow down the temp in one or two days...only for fun i love see big crystals.
i do this a few times..and no problem.. maybe is something more in the product before the purification that react
thanks man sorry all questions..
- By Mr Good Cat
Now I have 100% evidence long time exposure of MDMA at high temperature affects the color.
I use different crystallization methods and it is not a problem for me to get pure white crystals. Normally it doesn't take a lot of time for heating, and crystals are perfect white.
But this time I tried to do something new for me just to make crystals bigger and more transparent: "Per aspera ad astra".
I used the same batch of pure white powder after ABE, as solution was ready it had the same color as usually, transparent slightly brownish. I left it on the hotplate for 10 hours, T mostly 40-70C.
Unfortunately, I did a mistake in my calculations, and my expectations were not met. As the result I had to re-crystallize all this batch. As I made my solution ready for re-crystallization, it was much worse then before.
Still it is open question, what it is. It could be carbon of carbolic acid. Also it could be a natural property of salt to get dark while heated: jewelers ofter use it, and heat stones for long time to change the color.
But I noticed the solution of MDMA HCL that was not purified with base extraction gets much more dark brown and even much more fast.
So, I believe, still there is presence of some side product (not a lot, may be 1-2%) that turns black while heated.
I use different crystallization methods and it is not a problem for me to get pure white crystals. Normally it doesn't take a lot of time for heating, and crystals are perfect white.
But this time I tried to do something new for me just to make crystals bigger and more transparent: "Per aspera ad astra".
I used the same batch of pure white powder after ABE, as solution was ready it had the same color as usually, transparent slightly brownish. I left it on the hotplate for 10 hours, T mostly 40-70C.
Unfortunately, I did a mistake in my calculations, and my expectations were not met. As the result I had to re-crystallize all this batch. As I made my solution ready for re-crystallization, it was much worse then before.
Still it is open question, what it is. It could be carbon of carbolic acid. Also it could be a natural property of salt to get dark while heated: jewelers ofter use it, and heat stones for long time to change the color.
But I noticed the solution of MDMA HCL that was not purified with base extraction gets much more dark brown and even much more fast.
So, I believe, still there is presence of some side product (not a lot, may be 1-2%) that turns black while heated.
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