SWIM is doing some MHRB extractions in a mason jar, using Noman's tek (with added sodium carbonate wash from Vovin's tek). For the first batch of mimosa soup 50g lye, 750ml water and 50g MHRB (shredded, but powdered in SWIM's blender) were used. after 3 Naphtha pulls were done the solvent was collected in another jar and put in SWIM's freezer.
The next day, he and I noticed a layer of small, nice looking white/translucent crystals coating the jar up to the level of the naphtha. He opened the jar and poured the solvent off, and we brought the jar to his house (up to this point we had been at another friend's house) but in the 2-3 minute car ride, all the crystals had melted. At this point he didn't really know what to do with his melted crystals so we put them in his freezer in the sealed jar to store them until we could attempt to retrieve them.
(My thoughts at this point are that opening the jar before it warmed to room temperature may have caused condensation on the inside which dripped onto the crystals. And at this point SWIM was unaware of the upside down jar trick to let the solvent drip out of the crystals so i am not surprised that the melting happened.)
SWIM then attempted to recrystallize the melted crystals in an eyedropper bottle by moving what he could of the melted crystals from the jar into the bottle. of course it was re-melting by the time he started to move it so he ended up with just a small amount of melted crystal goo in the bottom of the eyedropper bottle and some dripping down the sides. He put this in a heat bath and added solvent until all of it seemed to be dissolved (everything in the bottle had melted down to a liquid by the time SWIM was adding solvent so very little additional solvent was added)
After this he taped a piece of coffee filter over the top of the eyedropper bottle, and set it by his freezer for perhaps 6-8 hours, after which time he moved it into his freezer.
The next day SWIM found the eyedropper bottle had some crustier looking opaque slightly pinkish-white crystals in it. so he removed these and placed them on a coffee filter to dry them, but after a minute they began to melt onto the filter so he moved it into his freezer in an attempt to give himself time to figure out what to do.
Also during this time SWIM had put the naphtha from the first batch back into his precipitation jar and that into his freezer. After about 24 hours he noticed there was a layer of slightly more discolored crystals on the inside of the jar, similar to what we found after the first precipitation. I informed him about letting the jar sit upside down to let the solvent drip out of the crystals and he let it sit like this for over 30 hours (SWIM is afraid of unwanted attention to his project and works on it on a sporadic schedule that i am very frustrated by). it was my understanding from reading these forums that this is much longer than is needed for the solvent to drip out.
So SWIM and I attempted to dry out these crystals and retrieve them. We opened the jar, secured a coffee filter over the top to keep dust out, and placed it near his air conditioner so the airflow would hopefully help dry the crystals. we noticed some condensation forming on the inside and wiped it off with a paper towel. it stopped forming soon as (I assume) the jar warmed to room temp. After 15-20 minutes or so we saw no liquid building up in the bottom of the jar, so we started to get (a little too) hopeful of our apparent success, since all our other crystals had quickly melted within 2 or 3 minutes, even while still in SWIM's freezer with the door open.
But it was not to last, for the crystals soon did start to melt. when we first noticed a bit of liquid pooling in the bottom of the jar we poured it off into the container with the used solvent. it created a small layer under the solvent so i assume this was water that we poured out (it looked and behaved like the water did during the sodium carbonate wash). My thoughts are that condensation formed on the crystals and the water began to dissolve them.
What has SWIM been doing wrong?? he is getting very frustrated with these melting crystals and there seems to be no way that any of our freeze precipitated crystals will become stable as a solid.
Right now our plan is to consolidate the melted crystals in the precipitation jar and on the coffee filter, and attempt to properly recrystallize this mess, using evaporation instead of SWIM's freezer, into a stable crystal as evaporation is the only thing he hasn't tried to get some smokeable spice, and it makes sense to me that a crystal formed by evaporation at room temp would have an easier time staying solid than one formed in a freezer.
To conclude:
A) Is it likely that the condensation that may have gotten into the melted crystals on the first precipitation would have remained in it and screwed up his attempt to recrystallize?
B) by leaving only a coffee filter over the eyedropper bottle after dissolving the melted crystals and during their subsequent time in the freezer would also mess up the recrystallization by not having the container sealed?
C) any thoughts on trying to retrieve what is soaked into the coffee filter at this point by putting pieces of it which the crystals melted onto in with the rest of the goo when SWIM tries to redissolve (before decanting the naphtha off to be put into an evaporation container)? i am thinking the filter may hold an amount worth retrieving since it is the first precipitation of this batch.
D) He removed the little bit of water/melting crystal that we poured into the jar of used solvent and put it in a small glass to attempt to evaporate it. would this still yield the product (and whatever impurities are with it)? Is there a better way to salvage water that may have some spice dissolved in it? (Water could potentially dissolve DMT, right?)
E) Is there a way to produce stable crystals by freeze precipitating? how would one go about drying them while avoiding condensation problems and oxidization?
Or if you have any other thoughts about any other part of SWIM's procedure or the plan I would very much appreciate any input! He is following the tek well and the only problem seems to be retrieval of the freebase from the solvent. None of the teks i have read go into much detail about how the spice should be dried. Every crystal produced by SWIM that he's been wishing to smoke has just melted into goo within a few minutes.
I can post the result of the attempted recrystallization once it is done. but so far SWIM has tried what I have found on these forums and in the FAQ with no success. Please help him get some smokeable spice out of this!
The next day, he and I noticed a layer of small, nice looking white/translucent crystals coating the jar up to the level of the naphtha. He opened the jar and poured the solvent off, and we brought the jar to his house (up to this point we had been at another friend's house) but in the 2-3 minute car ride, all the crystals had melted. At this point he didn't really know what to do with his melted crystals so we put them in his freezer in the sealed jar to store them until we could attempt to retrieve them.
(My thoughts at this point are that opening the jar before it warmed to room temperature may have caused condensation on the inside which dripped onto the crystals. And at this point SWIM was unaware of the upside down jar trick to let the solvent drip out of the crystals so i am not surprised that the melting happened.)
SWIM then attempted to recrystallize the melted crystals in an eyedropper bottle by moving what he could of the melted crystals from the jar into the bottle. of course it was re-melting by the time he started to move it so he ended up with just a small amount of melted crystal goo in the bottom of the eyedropper bottle and some dripping down the sides. He put this in a heat bath and added solvent until all of it seemed to be dissolved (everything in the bottle had melted down to a liquid by the time SWIM was adding solvent so very little additional solvent was added)
After this he taped a piece of coffee filter over the top of the eyedropper bottle, and set it by his freezer for perhaps 6-8 hours, after which time he moved it into his freezer.
The next day SWIM found the eyedropper bottle had some crustier looking opaque slightly pinkish-white crystals in it. so he removed these and placed them on a coffee filter to dry them, but after a minute they began to melt onto the filter so he moved it into his freezer in an attempt to give himself time to figure out what to do.
Also during this time SWIM had put the naphtha from the first batch back into his precipitation jar and that into his freezer. After about 24 hours he noticed there was a layer of slightly more discolored crystals on the inside of the jar, similar to what we found after the first precipitation. I informed him about letting the jar sit upside down to let the solvent drip out of the crystals and he let it sit like this for over 30 hours (SWIM is afraid of unwanted attention to his project and works on it on a sporadic schedule that i am very frustrated by). it was my understanding from reading these forums that this is much longer than is needed for the solvent to drip out.
So SWIM and I attempted to dry out these crystals and retrieve them. We opened the jar, secured a coffee filter over the top to keep dust out, and placed it near his air conditioner so the airflow would hopefully help dry the crystals. we noticed some condensation forming on the inside and wiped it off with a paper towel. it stopped forming soon as (I assume) the jar warmed to room temp. After 15-20 minutes or so we saw no liquid building up in the bottom of the jar, so we started to get (a little too) hopeful of our apparent success, since all our other crystals had quickly melted within 2 or 3 minutes, even while still in SWIM's freezer with the door open.
But it was not to last, for the crystals soon did start to melt. when we first noticed a bit of liquid pooling in the bottom of the jar we poured it off into the container with the used solvent. it created a small layer under the solvent so i assume this was water that we poured out (it looked and behaved like the water did during the sodium carbonate wash). My thoughts are that condensation formed on the crystals and the water began to dissolve them.
What has SWIM been doing wrong?? he is getting very frustrated with these melting crystals and there seems to be no way that any of our freeze precipitated crystals will become stable as a solid.
Right now our plan is to consolidate the melted crystals in the precipitation jar and on the coffee filter, and attempt to properly recrystallize this mess, using evaporation instead of SWIM's freezer, into a stable crystal as evaporation is the only thing he hasn't tried to get some smokeable spice, and it makes sense to me that a crystal formed by evaporation at room temp would have an easier time staying solid than one formed in a freezer.
To conclude:
A) Is it likely that the condensation that may have gotten into the melted crystals on the first precipitation would have remained in it and screwed up his attempt to recrystallize?
B) by leaving only a coffee filter over the eyedropper bottle after dissolving the melted crystals and during their subsequent time in the freezer would also mess up the recrystallization by not having the container sealed?
C) any thoughts on trying to retrieve what is soaked into the coffee filter at this point by putting pieces of it which the crystals melted onto in with the rest of the goo when SWIM tries to redissolve (before decanting the naphtha off to be put into an evaporation container)? i am thinking the filter may hold an amount worth retrieving since it is the first precipitation of this batch.
D) He removed the little bit of water/melting crystal that we poured into the jar of used solvent and put it in a small glass to attempt to evaporate it. would this still yield the product (and whatever impurities are with it)? Is there a better way to salvage water that may have some spice dissolved in it? (Water could potentially dissolve DMT, right?)
E) Is there a way to produce stable crystals by freeze precipitating? how would one go about drying them while avoiding condensation problems and oxidization?
Or if you have any other thoughts about any other part of SWIM's procedure or the plan I would very much appreciate any input! He is following the tek well and the only problem seems to be retrieval of the freebase from the solvent. None of the teks i have read go into much detail about how the spice should be dried. Every crystal produced by SWIM that he's been wishing to smoke has just melted into goo within a few minutes.
I can post the result of the attempted recrystallization once it is done. but so far SWIM has tried what I have found on these forums and in the FAQ with no success. Please help him get some smokeable spice out of this!
