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freeze precip.. how long does it usually take? (SWIM don't wanna go to bed:)
- Thread starter lorax
- Start date
Usually overnight in the freezer. But depending on how much spice is dissolved it may take a couple of days. The naphtha should go cloudy after 2-3 hours in the freezer (always a good indication for the impatient ones!) then slowly those microcrystals will be getting bigger and bigger and bigger...!
histones
Rising Star
with a smaller expcted yeild it shouldnt take any longer than an hour or 2. 3 hours to be absoluely sure.
if you are freezing say 100ml.. let it precip, drain the NP then either save the NP for future extractions or evap it to see whats left. SWIM usually only finds .07g or less of oily yellow crystals you would aim to separate from the larger batch of spice anyway.
As Ronue said, if you are expecting a great yeild then let it sit longer,
if you are freezing say 100ml.. let it precip, drain the NP then either save the NP for future extractions or evap it to see whats left. SWIM usually only finds .07g or less of oily yellow crystals you would aim to separate from the larger batch of spice anyway.
As Ronue said, if you are expecting a great yeild then let it sit longer,
69ron
Esteemed member
This is how it goes for SWIM, "I slowly add a small amount of warm 55 C heptane to my impure DMT. I use just enough to dissolve all of it and no more. When the heptane cools down to room temperature it starts looking cloudy. I place it in the freezer and usually see white crystals within 1 hour."
It can happen in as little as 1 hour if the quantity is small and you used as little solvent as possible. Also heptane seems to work better than naphtha. Most people use too much solvent because they don’t warm it to 55 C before using it.
The more DMT you have, the more solvent you'll need, and the longer it will take to cool down.
The same thing works for freebase 5-HO-DMT (bufotenine) if ethyl acetate is used instead of naphtha or heptane. In this case heat the solvent to 70 C and dissolve the 5-HO-DMT in as little solvent as possible, and then place it in the freezer. You should see crystals in a few hours.
It can happen in as little as 1 hour if the quantity is small and you used as little solvent as possible. Also heptane seems to work better than naphtha. Most people use too much solvent because they don’t warm it to 55 C before using it.
The more DMT you have, the more solvent you'll need, and the longer it will take to cool down.
The same thing works for freebase 5-HO-DMT (bufotenine) if ethyl acetate is used instead of naphtha or heptane. In this case heat the solvent to 70 C and dissolve the 5-HO-DMT in as little solvent as possible, and then place it in the freezer. You should see crystals in a few hours.
If you are freeze precipitating an extraction, not re-crystallizing, I wouldn't try leaving it in the freezer for only an hour or so.
Try at least 24 hours.
More if you can be patient.
In the extractions I've done (basically following "Vovin's" tech) I've never used more than 150g of MHRB, My yield is usually between .75mg to .100mg of clear to white crystals, straight from the freezer!!
I do three Naptha pulls on the basified (13-14Ph) bark solution. The first one I use 100ml of Naptha warmed to 130-140f degrees. On the second & third pulls, only 75ml of warm Naptha is used.
When all three pulls are finished, I add them together (usually 450m-to-500ml total) and do a sodium carbonate wash on it. One wash using 20ml of room temp distilled water & a tiny pinch of Sodium Carbonate, the second & third washes use 20ml of room temp distilled water only.
The washed Natha is left to sit in a beaker, at an angle, for 5-to-10 minutes so any water that may have snuck out of the seperatory funnel with the Naptha can collect together at the bottom. This makes it easier for the water to be removed, before/while using a pipette to move the alka-loaded Naptha from the breaker, in equal amounts, into three small jelly jars.
I put a piece of plastic wrap over the top of the jars, then screw the lids on tight, to make sure no oxygen gets in there while precipitating.
The jars are then put into the back of the refrigerator for about 12 hours, then they are moved into the back of the freezer and left untouched for at least 24 hours. I take a look at the jar(s) every 8 to 10 hours to see when the crystals are no longer falling out of the Naptha, I leave them for at very least an hour or two after that to be sure. Then I filter them out with a Buchner filter & let dry completely!!
BTW:
If you'd like larger crystals, instead of a bunch of smaller shards, once the jars are moved to the freezer, leave them in there for only like 12 hours or so. Then move them back to the fridge for an hour, maybe an hour & a half (you'll need to watch this process very closely, too be sure your not re-dissolving all of your spice!). Then out, on to the counter top for 30 minutes and back into the fridge for an hour or so, then back to the freezer for 4-to-6 hours and back to the fridge, etc...etc...
Repeat these steps, freezer > fridge > room temp > fridge > freezer > fridge > room temp > fridge > freezer, over & over a number of times and your tiny, shard-like crystals will start to form larger & larger crystals!!
Do not swirl the Naptha, or move the jar around too much!!
When the smaller shards first start to bond to a larger crystal, until they have been warmed & cooled a few times, it is very easy for them to be "knocked off" by swirling the liquid around too much or something similar.
It is important to not disturb the crystal formations while moving the jar!!
This works because as the Naptha warms up slowly, little by little, the smaller crystals will "melt" back into the solvent but the bigger crystals take much longer to fully dissolve.
So as the solvent is then cooled back down to freezing temps, the DMT is squeezed back out and the new, smaller shards will cling to the bigger, already formed crystals and grow onto them, causing large, beautiful crystals!! Of course you have to be patient enough to repeat this process a few times a day (and/or night) for a few weeks.
This technique does take some time, but is worth it!! This method of freeze precip also gets pretty much all of the alkaloids out of the Naptha, like evaporating does. Warming & cooling over & over will squeezed out more of the spice than just freezing it one time & filtering!!
When I put my 3 jars of alka-loaded Naptha in the freezer for precipitation, I usually choose one jar to stay in and grow large crystals. The other two are removed after 1 to 2 days, and the spice is filtered out, but the third jar goes through the above process to grow some larger crystals that I keep for special occasions like the S.H.E., etc...
It amazes me, the beautiful fractal formations that grow simply from modifying the temp of the solvent!!
If you are doing a re-crystallization, this can go much, much quicker. 69ron had some good advice there!! As a general rule, I myself try to leave the alka-loaded Naptha in the freezer as long as I can. This usually amounts to 24-to-48 hours for the first two jars anyway!!
Good luck!!
WS
Try at least 24 hours.
More if you can be patient.
In the extractions I've done (basically following "Vovin's" tech) I've never used more than 150g of MHRB, My yield is usually between .75mg to .100mg of clear to white crystals, straight from the freezer!!
I do three Naptha pulls on the basified (13-14Ph) bark solution. The first one I use 100ml of Naptha warmed to 130-140f degrees. On the second & third pulls, only 75ml of warm Naptha is used.
When all three pulls are finished, I add them together (usually 450m-to-500ml total) and do a sodium carbonate wash on it. One wash using 20ml of room temp distilled water & a tiny pinch of Sodium Carbonate, the second & third washes use 20ml of room temp distilled water only.
The washed Natha is left to sit in a beaker, at an angle, for 5-to-10 minutes so any water that may have snuck out of the seperatory funnel with the Naptha can collect together at the bottom. This makes it easier for the water to be removed, before/while using a pipette to move the alka-loaded Naptha from the breaker, in equal amounts, into three small jelly jars.
I put a piece of plastic wrap over the top of the jars, then screw the lids on tight, to make sure no oxygen gets in there while precipitating.
The jars are then put into the back of the refrigerator for about 12 hours, then they are moved into the back of the freezer and left untouched for at least 24 hours. I take a look at the jar(s) every 8 to 10 hours to see when the crystals are no longer falling out of the Naptha, I leave them for at very least an hour or two after that to be sure. Then I filter them out with a Buchner filter & let dry completely!!
BTW:
If you'd like larger crystals, instead of a bunch of smaller shards, once the jars are moved to the freezer, leave them in there for only like 12 hours or so. Then move them back to the fridge for an hour, maybe an hour & a half (you'll need to watch this process very closely, too be sure your not re-dissolving all of your spice!). Then out, on to the counter top for 30 minutes and back into the fridge for an hour or so, then back to the freezer for 4-to-6 hours and back to the fridge, etc...etc...
Repeat these steps, freezer > fridge > room temp > fridge > freezer > fridge > room temp > fridge > freezer, over & over a number of times and your tiny, shard-like crystals will start to form larger & larger crystals!!
Do not swirl the Naptha, or move the jar around too much!!
When the smaller shards first start to bond to a larger crystal, until they have been warmed & cooled a few times, it is very easy for them to be "knocked off" by swirling the liquid around too much or something similar.
It is important to not disturb the crystal formations while moving the jar!!
This works because as the Naptha warms up slowly, little by little, the smaller crystals will "melt" back into the solvent but the bigger crystals take much longer to fully dissolve.
So as the solvent is then cooled back down to freezing temps, the DMT is squeezed back out and the new, smaller shards will cling to the bigger, already formed crystals and grow onto them, causing large, beautiful crystals!! Of course you have to be patient enough to repeat this process a few times a day (and/or night) for a few weeks.
This technique does take some time, but is worth it!! This method of freeze precip also gets pretty much all of the alkaloids out of the Naptha, like evaporating does. Warming & cooling over & over will squeezed out more of the spice than just freezing it one time & filtering!!
When I put my 3 jars of alka-loaded Naptha in the freezer for precipitation, I usually choose one jar to stay in and grow large crystals. The other two are removed after 1 to 2 days, and the spice is filtered out, but the third jar goes through the above process to grow some larger crystals that I keep for special occasions like the S.H.E., etc...
It amazes me, the beautiful fractal formations that grow simply from modifying the temp of the solvent!!
If you are doing a re-crystallization, this can go much, much quicker. 69ron had some good advice there!! As a general rule, I myself try to leave the alka-loaded Naptha in the freezer as long as I can. This usually amounts to 24-to-48 hours for the first two jars anyway!!
Good luck!!
WS
If your solution is saturated enough to precip, but not WAY saturated, it can take days for it all to fall out. If the solvent stays cloudy for longer than a few hours with nothing falling out, this is likely the case and my friend usually just shoves the jar into the back of the freezer and forgets about it for awhile.
69ron
Esteemed member
Basically 3 things cause problems in freeze precipitation:
1) Too much solvent is used. This is the most common problem. This can cause it to fail to precipitate. Even at freezing temperatures, DMT is soluble in naphtha and heptane, but just very poorly soluble. If you dissolve the DMT in 55 C solvent, and it doesn’t get cloudy after cooling down to room temperature, you used too much solvent. Evaporate some of it away.
2) The temperature is not low enough. Make sure your freezer is at 0 F or lower.
3) There are too many impurities present. Make sure you clean up your extract. Too many impurities can prevent crystallization.
1) Too much solvent is used. This is the most common problem. This can cause it to fail to precipitate. Even at freezing temperatures, DMT is soluble in naphtha and heptane, but just very poorly soluble. If you dissolve the DMT in 55 C solvent, and it doesn’t get cloudy after cooling down to room temperature, you used too much solvent. Evaporate some of it away.
2) The temperature is not low enough. Make sure your freezer is at 0 F or lower.
3) There are too many impurities present. Make sure you clean up your extract. Too many impurities can prevent crystallization.
atheistpeace
Rising Star
swim did a 24 hr freeze precip once and got the spice, put the jar of naphtha back in freezer and checked 5 days later and there was an extra 300+mg in there.