I have recently recrystallized all my spice using the slow water crystallization method. It is totally awesome, so much smoother! It smells a lot less than naphtha-crystallized DMT too.
It took me some time to master, so I'll add my experiences here. These are in part just a recollection of things discovered by other people in this thread, but also a tiny experiment.
- I saturate some water with sodium carbonate, put this in the fridge to precip sodium carbonate that would otherwise precip later, then filter and use this solution.
- I then add this to my dissolved fumarates. When done slowly the impurities all stick to the bottom! If you decant the solution into another container the rest that will precip is very white! Of course the impurities that stick to the bottom still have quite a bit of DMT in them, but you can separate light yellow DMT into yellow and white DMT
. I've done this numerous times, and most of the time this works perfectly.
An example, I used some dark DMT and decanted, leaving me with dark freebase in one container and this in the other:
- Definitely wait the full 5 days or longer, water crystallization takes it's sweet time. Freezing and thawing your solution will give some more crystals. Even after waiting a week and freeze-thawing there was still DMT left in the carbonate solution, a small but significant amount (5-10%). I've had this every time. Do NOT throw your water away. Instead pull again with naphtha to retrieve the last bit of DMT.
- The idea of letting your jar warm to room temperature is a good one, I do this every time it ensures no sodium carbonate crystals are stuck between your DMT.
- However, without vacuum filtration, there is a lot of sodium carbonate contamination if you don't wash your crystals after collecting them. This is no problem, only if you want purity. I found contrasting information on how to further clean this contamination off my crystals.
Water washed are advised, which left me wondering because DMT has a pKa of 8,68, so if tap water was used part of the DMT would be in salt form and thus dissolve, I thought. Can someone please elaborate if this thought is correct?
An ammonia wash apparently would dissolve part of my DMT. Again, what is the proposed mechanism behind this? When using a pH 11 solution of ammonia, how can DMT dissolve? Ammonia would be the perfect base because it evaporates away.
A sodium carbonate wash would leave me with contamination because a significant amount of sodium carbonate is needed to get the washing water basic enough.
A sodium hydroxide wash is never mentioned because it is a strong base and people prefer not to have this in their product, even though a minute quantity would be sufficient to get the water basic enough.
This was all very unclear to me, and since I love water crystallized DMT dissolving the product in IPA/acetone and filtering out the carbonate contamination was not an option.
I prepared 4 containers with 15 ml of solution in them: 1 with a pH 11 solution of sodium carbonate, 1 with a pH 11 solution of ammonia, 1 with a pH 11 solution of sodium hydroxide, and 1 with 15 ml tap water (which is pH 7,8 here). PH 11 was arbitrarily chosen because virtually all DMT is in freebase form then.
In every one of these containers I put 500 mg of fairly pure, water crystallized DMT with sodium carbonate contamination. The pH of the tap water container rose to 10,4 upon adding the DMT. The containers were left for an hour in which they were occasionally stirred, then the DMT was filtered out and weighed.
The results: DMT from all containers weighed in at about 440 mg, only a few mg difference. It seems the ammonia did not have a detrimental effect on the yield.
One question remains: the excess sodium carbonate raised the pH of the tap water container to 10,4. If pure DMT is put in tap water, won't part of it dissolve?
Before that question is answered I'll stay on the safe side and use pH11 ammonia solution to wash my crystals.
It took me some time to master, so I'll add my experiences here. These are in part just a recollection of things discovered by other people in this thread, but also a tiny experiment.
- I saturate some water with sodium carbonate, put this in the fridge to precip sodium carbonate that would otherwise precip later, then filter and use this solution.
- I then add this to my dissolved fumarates. When done slowly the impurities all stick to the bottom! If you decant the solution into another container the rest that will precip is very white! Of course the impurities that stick to the bottom still have quite a bit of DMT in them, but you can separate light yellow DMT into yellow and white DMT
. I've done this numerous times, and most of the time this works perfectly. An example, I used some dark DMT and decanted, leaving me with dark freebase in one container and this in the other:
- Definitely wait the full 5 days or longer, water crystallization takes it's sweet time. Freezing and thawing your solution will give some more crystals. Even after waiting a week and freeze-thawing there was still DMT left in the carbonate solution, a small but significant amount (5-10%). I've had this every time. Do NOT throw your water away. Instead pull again with naphtha to retrieve the last bit of DMT.
- The idea of letting your jar warm to room temperature is a good one, I do this every time it ensures no sodium carbonate crystals are stuck between your DMT.
- However, without vacuum filtration, there is a lot of sodium carbonate contamination if you don't wash your crystals after collecting them. This is no problem, only if you want purity. I found contrasting information on how to further clean this contamination off my crystals.
Water washed are advised, which left me wondering because DMT has a pKa of 8,68, so if tap water was used part of the DMT would be in salt form and thus dissolve, I thought. Can someone please elaborate if this thought is correct?
An ammonia wash apparently would dissolve part of my DMT. Again, what is the proposed mechanism behind this? When using a pH 11 solution of ammonia, how can DMT dissolve? Ammonia would be the perfect base because it evaporates away.
A sodium carbonate wash would leave me with contamination because a significant amount of sodium carbonate is needed to get the washing water basic enough.
A sodium hydroxide wash is never mentioned because it is a strong base and people prefer not to have this in their product, even though a minute quantity would be sufficient to get the water basic enough.
This was all very unclear to me, and since I love water crystallized DMT dissolving the product in IPA/acetone and filtering out the carbonate contamination was not an option.
I prepared 4 containers with 15 ml of solution in them: 1 with a pH 11 solution of sodium carbonate, 1 with a pH 11 solution of ammonia, 1 with a pH 11 solution of sodium hydroxide, and 1 with 15 ml tap water (which is pH 7,8 here). PH 11 was arbitrarily chosen because virtually all DMT is in freebase form then.
In every one of these containers I put 500 mg of fairly pure, water crystallized DMT with sodium carbonate contamination. The pH of the tap water container rose to 10,4 upon adding the DMT. The containers were left for an hour in which they were occasionally stirred, then the DMT was filtered out and weighed.
The results: DMT from all containers weighed in at about 440 mg, only a few mg difference. It seems the ammonia did not have a detrimental effect on the yield.
One question remains: the excess sodium carbonate raised the pH of the tap water container to 10,4. If pure DMT is put in tap water, won't part of it dissolve?
Before that question is answered I'll stay on the safe side and use pH11 ammonia solution to wash my crystals
.