"MY" MDMA freebase crystallization

[Davidrobinson]

It should be ok because you crashed ot out in acetone. More acid just makes more impurities.
Did you get big crystals from pouring the hot acidified freebase into cold acetone?

 

[btcboss2022]

It should be ok because you crashed ot out in acetone. More acid just makes more impurities.
Did you get big crystals from pouring the hot acidified freebase into cold acetone?

oscar412When I did It in past at 120C yes I got Big crystals now at 130C I get shiny powder

Thanks.

 

[kharpa177]

When I did It in past at 120C yes I got Big crystals now at 130C I get shiny powder

Thanks.

btcboss2022hello bro, could you help me... I wanted to crystallize this freebase... after acidifying the freebase with acid... heat the freebase to 110° and throw it in the cold acetone And so on? or would you have to mix the freebase with some solvent before heating?

 

[btcboss2022]

hello bro, could you help me... I wanted to crystallize this freebase... after acidifying the freebase with acid... heat the freebase to 110° and throw it in the cold acetone And so on? or would you have to mix the freebase with some solvent before heating?

kharpa177Bring it to PH-4.5/5 heat it to 130C and throw it in 5 times freebase volume cold acetone. Filter it, wash it, dry it, solve in water 1gr:1ml and heat it to 108C to recrystallize.

 

[kharpa177]

Bring it to PH-4.5/5 heat it to 130C and throw it in 5 times freebase volume cold acetone. Filter it, wash it, dry it, solve in water 1gr:1ml and heat it to 108C to recrystallize.

btcboss2022acidifies the free base without solvent ? throw the acidified freebase into the cold acetone after the end ... when I acidify the freebase it drops the ph very quickly and the freebase turns pink is this normal ??

 

[kharpa177]

Bring it to PH-4.5/5 heat it to 130C and throw it in 5 times freebase volume cold acetone. Filter it, wash it, dry it, solve in water 1gr:1ml and heat it to 108C to recrystallize.

btcboss2022do crystals form after dropping warmed and acidified freebase into cold acetone? that's what i wanted to know

 

[btcboss2022]

do crystals form after dropping warmed and acidified freebase into cold acetone? that's what i wanted to know

kharpa177In that step after Heat at 130c small crystals(like White powder) forms when pouring and stir It in Freeze acetone.

 

[kharpa177]

In that step after Heat at 130c small crystals(like White powder) forms when pouring and stir It in Freeze acetone.

btcboss2022Is it normal for the solution to turn pink? .. these crystals appeared I made 15g of pmk

 

[btcboss2022]

Is it normal for the solution to turn pink? .. these crystals appeared I made 15g of pmk

kharpa177What step is this one?

 

[btcboss2022]

Now I'm totally focused in MDMA production and I saw that for MDMA you get more beautiful shards when a very little portion of water is remaining during the crystallization process so the heating temp is better to leave it in 108C possibly less I will test it and update it.
Another point to update is the time of crystallization in acetone I made different tests and when acetone arrives again to -2C -5C no more crystals are generated so the waiting time could be reduced until that moment.
Thanks.

 

[Mr Good Cat]

Now I'm totally focused in MDMA production and I saw that for MDMA you get more beautiful shards when a very little portion of water is remaining during the crystallization process so the heating temp is better to leave it in 108C possibly less I will test it and update it.
Another point to update is the time of crystallization in acetone I made different tests and when acetone arrives again to -2C -5C no more crystals are generated so the waiting time could be reduced until that moment.
Thanks.

btcboss2022As I got from your description, we evaporate the excess of water until we get a saturated solution of MDMA in water under the temperature 108C.
Does the speed / intensity of the heating (evaporating) make any difference?
And another question: what is approx volume of this saturated solution ready for cristallization if we are working with 100 gr of MDMA HCL?

 

[kharpa177]

This is what i get

mocnykutashello bro, could you help me... I wanted to crystallize this freebase... after acidifying the freebase with acid... heat the freebase to 110° and throw it in the cold acetone And so on? or would you have to mix the freebase with some solvent before heating?

 

[kharpa177]

This is what i get

mocnykutaswhat would be the correct ph of mdma freebase after extracted with xylene? ph 6 ?

 

[kharpa177]

This is what i get

mocnykutaswhat would be the correct ph of mdma freebase after extracted with xylene? ph 6 ?

 

[kharpa177]

This is what i get

mocnykutasdid you heat your acidified free base with distilled water and give these crystals? could you explain me better?

 

[kharpa177]

This is what i get

mocnykutasdid you heat your acidified free base with distilled water and give these crystals? could you explain me better?

 

[kharpa177]

This is what i get

mocnykutasCould you tell me how you crystallized your freebase? had to warm up your freebase?

 

[kharpa177]

after weeks studying this crystallization managed to obtain white crystals mdma \0/

 

[FredDurst]

8. Solve the powder in distilled hot water(1gr/1ml).

9. When all the powder is solved Heat the mixture until 112C with some stirring and throw It fast into the cristallization bucket choosen.

btcboss2022Hi mate. I have a few questions about this part of your procedure

Do you leave the mixture at 112c until water boils away or just get to that temp and pour straight in the bucket?

In the bucket you have cold acetone again?

Do you not loose loads of product in the remaining water?

Thanks

 

[FredDurst]

Hi mate. I have a few questions about this part of your procedure

Do you leave the mixture at 112c until water boils away or just get to that temp and pour straight in the bucket?

In the bucket you have cold acetone again?

Do you not loose loads of product in the remaining water?

Thanks

FredDurst

8. Solve the powder in distilled hot water(1gr/1ml).

9. When all the powder is solved Heat the mixture until 112C with some stirring and throw It fast into the cristallization bucket choosen.

 

[kharpa177]

Hi mate. I have a few questions about this part of your procedure

Do you leave the mixture at 112c until water boils away or just get to that temp and pour straight in the bucket?

In the bucket you have cold acetone again?

Do you not loose loads of product in the remaining water?

Thanks

FredDurstthere are so many methods that even people are confused... I used this method and it doesn't work... some say crystallization at room temperature with cold acetone... others say it's by heating

 

[Mr Good Cat]

there are so many methods that even people are confused... I used this method and it doesn't work... some say crystallization at room temperature with cold acetone... others say it's by heating

kharpa177I used this method offered by TS with the product sold by TS on 108C. This method works and crystals grow, but neither big nor clean. The percentage of the pollutants was so huge that all my solution at the end of evaporation was completely black. The crystals themselves were from grey to black. I'm not sure if this product had any preliminary purification. Obviously, such product is not acceptable for consumption.
Then, with such load of impurities the crystals start to grow around all these impurities as nucleation centers.
So I had to finish it with acid base extraction and the result is good.
So the method works but not undoubtedly. And by a funny coincidence, this does not apply to the product sold by the author.
Photos of the cleanest part of crystals, turned to the base and most dirty part of crystals after they were smashed and washed with acetone.
Still hesitating, shall I try to grow big crystals or leave it as it is in pure white powder form.

 

[btcboss2022]

I used this method offered by TS with the product sold by TS on 108C. This method works and crystals grow, but neither big nor clean. The percentage of the pollutants was so huge that all my solution at the end of evaporation was completely black. The crystals themselves were from grey to black. I'm not sure if this product had any preliminary purification. Obviously, such product is not acceptable for consumption.
Then, with such load of impurities the crystals start to grow around all these impurities as nucleation centers.
So I had to finish it with acid base extraction and the result is good.
So the method works but not undoubtedly. And by a funny coincidence, this does not apply to the product sold by the author.
Photos of the cleanest part of crystals, turned to the base and most dirty part of crystals after they were smashed and washed with acetone.
Still hesitating, shall I try to grow big crystals or leave it as it is in pure white powder form.

View attachment 12225 View attachment 12226

Policja PolskaI think that no other way to show exactly my process that making a video as soon I come back to work again, will be a no professional video and I don't know when I will do it yet. But many doubts from many people and other ones not doing the steps correctly.

 

[Mr Good Cat]

i had one set up test based on dry ipa and xylene... i think i have to work on the one with xylene.... will do right now.. tbc..,

bblancoto be honest, I really like the method of crystallization of oversaturation solutions MDMA HCl + water, described by btcboss.
I did try it and it works perfectly if certain conditions applied. This shall be really calm place, without air flows and vibrations.
Once I did the stupidity - turned on the washing machine while crystallization was going on. As the result crystals grown not so nice and a kind of "small"

 

[Mr Good Cat]

shulgin writes this:

"The actual form that the final salt takes depends upon the temperature and concentration at the moment of the initial crystallization. It can be anhydrous, or it can be any of several hydrated forms. Only the anhydrous form has a sharp mp; the published reports describe all possible one degree melting point values over the range from 148-153 ° C. The variously hydrated polymorphs have distinct infrared spectra, but have broad mps that depend on the rate of heating. "

bblancocheck this picture, pls., it explains the importance of correct temperature pretty well.
if temperature of the solution grows, the saturation grows as well.
you can also read about Raoult's laws. briefly, is says: boiling temperature of the solution depends on the molar quantity of saturated salt. so, this temperature 108C suggested by @btcboss2022 probably reffers to the highest point of the "size" graph.
on the other side, the impurities become crystallization centers as well, so "dirty" solution will not bear you big crystals.

 

[btcboss2022]

Hi mate. I have a few questions about this part of your procedure

Do you leave the mixture at 112c until water boils away or just get to that temp and pour straight in the bucket?

In the bucket you have cold acetone again?

Do you not loose loads of product in the remaining water?

Thanks

FredDurstI changed now the last part of re-crystallization with water to 108C at this temp no so much water remaining and the liquid remaining after crystallization must be used in the next batch or reheated. In water recrystallization part no acetone in the bucket that is the previous step at 130C.

 

[Mr Good Cat]

Do you not loose loads of product in the remaining water?

FredDurstLast time, when re-crystallizing dry salt with this 108C method I lost 5.4% of dry weight.

 

[Mr Good Cat]

Last time, when re-crystallizing dry salt with this 108C method I lost 5.4% of dry weight.

Policja PolskaSorry, I forgot to count the leftovers from acetone. So, it is much less: 2.6% lost, that's not bad at all.