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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.
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
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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
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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
↑View previous replies…
Policja Polskashulgin 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. "
Policja Polskai 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"
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.
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- By bblanco
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
"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. "
- Joined
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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
- Joined
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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..,
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"
- Joined
- Jan 6, 2023
- Messages
- 281
- Reaction score
- 110
- Points
- 43
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. "
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.
![SMGXYkfisz SMGXYkfisz](https://bbgate.com/data/attachments/13/13325-d42ad55f286b15217e09497b09d03e37.jpg)