OK, so I have a possibly odd question. Has anyone had to do a freeze precip more than once on a given batch of pulls? I did an extract on 175g of MHRB using the Max Ion tek. I used slightly more than 50ml for each pull and ended up with about 450ml of naptha in the end. When I went to evap to concentrate it, it went milky to the point of not being able to see through about 3/4" of naphtha (I use a small pyrex dish) in only about 15 minutes. Into the freezer it went this past Wednesday.

Forward to today. I pull the dish out of the freezer and am greeted by a nice, thick layer of white crystal goodness and begin pouring off the naphtha. Once it's poured off and I place the dish upside down to drip, I look at the poured off naphtha. It's slightly cloudy. Pardon? Really? After getting the crystal-laden dish setup with a fan blowing on it, I put the other dish to evap and see if it will go milkier. Holy Dinah! It is. After only 10 minutes it's quite milky yet again. This seems like craziness, not that I'm complaining at all though of course.

So... Has anyone else had this happen? Is it a result of the smaller dish? It's only 6.5" x 4.5". Can dmt crystals only form so thick a layer then they won't precip out any more? Should I be either using a bigger dish or multiple smaller ones to give more surface area for the crystals to fully precip out?

Here's the main dish pre-scraping:


Yield so far:

It has nothing to do with surface area of the bottom. In fact, smaller surface area might be better since it would mean a higher chance of the particles swirling past and crashing into nice, big piles of sediment, and landing.

The DMT particles are suspended in the solvent. The cold makes the solvent incapable of containing as much DMT and causes them to sink down. They form sediment (crystals) at the bottom of the container.

But you're not going to get 100% of the DMT out via freeze precipitation. It's just not possible. Some will always stay in the solvent, since it retains some solubility even in cold.

The longer you keep it in the freezer, the more sediment you will get, of course. ~5 hours will give some sediment (good to know if you want some quick crystals, and then putting it back in the freezer). 24 hours will give a lot. 48 will give maybe 50% more. etc.

It's common to freeze precip the same exact solvent twice: First for 24 hours, then pick up the crystals, and then freeze it again for 24-48 hours for some more crystals.

My suggestion is to re-use that same solvent like 3-6 times for future extractions, so that nothing goes to waste. And then when the solvent isn't good anymore (when it's so full of particles that it's no longer giving you big pulls even from brand new bark extractions), it's time to finally evaporate all of that "spent" solvent so that it releases everything.

PS: Your "cloudiness" test isn't completely proper. Cloudiness is not to be expected whatsoever at room temperature. At room temperature, the DMT is a transparent liquid that is completely diluted inside the solvent, meaning that pulls are pretty much completely transparent apart from some slight yellowish color. The clouds only come when the solvent has been freezing for a few hours so that that the liquid DMT particles have frozen back into opaque solids and have started clumping together inside the solvent, thus making it appear thicker/cloudier. I guess some evaporation may force the liquid to become cloudier even at room temperature, but it's not a good test at all. Even very saturated liquid will be almost transparent at room temperature.

PPS: For future extractions I suggest you use less solvent instead of wasting it via evaporation. For 175 grams of bark you should calculate pull-size as 0.5:1, half the bark weight. So that's 0.5*175 = 87.5 milliliters per pull. For three pulls that's 262.5 milliliters. At that solvent:bark ratio, your solvent will already be saturated and you won't have to evaporate any of it. You used 450 milliliters of solvent which is a truckload (70% more).

Thanks for the info Samadeus. You're the first person I've ever seen say to do a second freeze. I wonder how much spice I've lost in previous extracts? Ahh well.

You're welcome!


The need for a second freeze depends on how long your initial freeze is.

People doing 24 hour extracts must always freeze again after that since there's going to be a lot more left in the solvent. In that case, you usually get like 70% of the total weight in the first 24 hours, and another 30% in the second 24-48 hour period. Here's an example: 430mg on the first freeze, and 200mg on the second freeze, of the exact same solvent.

People who always do multiple days of freezing will have more time for the sediment to settle and therefore won't get very much if they try to freeze it again after that. There will only be a few extra crystals, since solvent always contains a little bit of DMT even at cold temperatures, so some more of it will probably still fall out. But most of the freeze-"precipitable" (hehe) portion will have fallen out during the first few days! I'd say 2 or 3 days is going to get most of the freezable portion out.

So if you already did multi-day freezes every time, you haven't lost much freezer-wise!


In either case, always remember to evap everything away when the solvent has finally served its full life (3-6 extractions), so that you get all the remaining product out of there.


PS: Speaking of "lost DMT". A lot of newbies throw away their black water after their first few pulls are done. That makes me sad. There's always a lot more DMT in there, since there's no way your solvent has made contact with *all* of the DMT-containing water *even* if you thoroughly mixed!
There are two ways to extract all of the goodness from the water:
- Either do 5 pulls right away and get most of it thanks to the sheer number of pulls. But then you have to evap away solvent since you'll have way too much solvent in your jar. So that's wasteful.
- The second way is better: Do 3 pulls on day 1, freeze precip that for 24 hours, take out some crystals, freeze precip it again for 24 hours, take out the rest of the crystals, and then you just re-use the exact same solvent again and split the solvent amount into 2 bigger (therefore easier) pulls, and freeze precip that one last time.


Also, do heated pulls in the future if you haven't tried that already. It means you achieve supersaturated solvent much easier. Heat = allows solvent to hold more DMT. Cold = allows solvent to hold less DMT. By heating the solvent jar and mixing jars under the hot water tap, you'll get more DMT per pull.

the only thing freezing does is lower the solubility of a solute in a solvent; multiple cycles of freezing may grow larger crystals, but that isn't an increase in yield.

If you freeze at -20°C for 12h there's almost no DMT dissolved left in your naphta but you can lose some fine cristals floating around when you pour the solvent off.

The above is completely incorrect and beyond wrong. It's the kind of misinfo that could cause newbies to read it and throw away massive yields, believing they've got most of the product after the ridiculously low freeze time of just 12 hours. Please don't mislead people...

Most European freezers are at -18C, and here's an example yield (mentioned above):

430mg DMT after 24 hours. And then it went back in the freezer for 48 more hours (so 72 in total) and yielded another 200mg from the same solvent.

After only 12 hours you would only have like ~30% of the total DMT available! The other 70% is still trapped in the solvent.


Your second statement is equally wrong, "after a freeze precipitation there is almost no DMT left in the solvent."

That's completely wrong. Solvent is still solvent even when cold. The coldness reduces its carrying capacity for DMT but it will still contain a big amount, especially if you have lots of solvent (more surface area). The only way to get *all* DMT out of the solvent is to evaporate it. But as I explained earlier, it's wasteful to evaporate it. Just re-use the same solvent a few times and *then* evaporate it after 3-6 uses.

Oh and you will know when to evaporate it: At a certain point the solvent is so full of plant oils and DMT that it is no longer suitable for new extractions since it can't carry much new DMT anymore. So when your future pulls are giving much smaller yields than expected, that "spent" solvent has finally become useless for new extracts and should be evaporated. This happens after like 3-6 reuses.

I have to say that what you wrote hurt my ego (teh famous ) the way you did.

I said what i said because during the first extaction i did 1 year ago, i put the naphta in the freezer in the evening and in the morning (so ~12hours)i poured the solvent out and for the sake of my knowledge i evaporated it to see how much magic was still in it. In my memory, there was not much so after that it was a fact in my mind.

After your claim , i thought omg, i'm bad, because spreading misinformation is something i try to avoid and i hate that when another does it.
But my ego was telling me (i try to not listen it to much but i'm weak ) don't let him put you down it's disrespectfull. So i did an experiment.

The rest of my last batch needed a re-x (not realy in fact but you know...) and i wanted to clean few containers with an "unscrapeable" coat of DMT (i'm no-waste-man !). I did it and the result was ~50ml of hot naphta. I let it at room temp for 1h then put it in the fridge @ 5°C for 2h and finaly in the freezer @ -20°C for less than 7h (6h and 35min to be anal). The total is ~13h. Then i poured the naphta out and evaporate 4/5 of it (the remaining was ~10ml) and put it back in the freezer for 10h and as there was almost nothing in it i totaly evaporated it. The numbers :
After 13h i got 440mg
After 10h more i had ~5mg
After evaporating (i couldn't pick it up because of the shape of the container so i guestimate it) ~10mg.
I did my math and the result is : after 13h i got 96,7% of DMT from the naphta and, consequently, 3,3% was still in the solvent.

My conclusion is : i repeat what i said, after 12h in a freezer @-20°C there is almost no DMT dissolved in the naphta. At -20°C DMT is almost insoluble in naphta.


What can happen : if you cool your solvent to fast, DMT won't form big cristals but tiny ones and they will set up in the bottom slowly making a coat of DMT. If you don't wait enough, they still float in suspension and you pour them out with the solvent.

And btw, instead of evaporate the old re-used naphta it's better to salt it because you don't end up with a bunch of oil and fat.



^This is the result of my ego, i think it's time to try to kill it with my fresh new bach of white and shinny x-tals


Edit : it didn't work. But i did some new weird throat sounds

I can settle this argument between you. The answer is that you are both right.

It totally depends on the method of crystallization. Gradual cooling is recommended, since it takes less time and gives bigger crystals.

To understand why this happens, people need to understand what actually happens to a solute (DMT in this case) when placed in a solvent.


What is heat and why does hot solvent pull more DMT?

First, people need to know why hot solvents dissolve particles better than cold solvents: Heat-energy is what breaks apart the molecular bonds in the crystal lattice of the solute (in this case DMT), so that the crystals break down into their individual molecules, which then become light enough to bond to the solvent instead. This is why hotter solvent can hold more solute (DMT), and why hot pulls are much, much better than cold pulls.

In fact, heat itself is nothing more than the kinetic energy of vibrating (dancing) molecules. The faster/more forcefully they vibrate, the "hotter" it is. But the atoms themselves don't "know" that they're "hot" or "cold". They're simply vibrating. "Hotter" is actually just a word for "vibrating so forcefully that they collide into and rip apart any other molecular structures they come into contact with". When we touch something "hot", its interaction with our body is what we perceive as the feeling of "heat".

And that interaction is simple: Collisions! The high vibrational energy of a heated material will cause it to smash into the atoms of a lower-temperature material (or vice versa), and that's what you feel as the pain of "hot" things. It's just the atoms smashing into each other and ripping each other's structural integrity apart.

This can be seen if you lower hot iron into cold water. There will be violent bubbling. But as soon as the atoms in the two different-temperature materials have reached the same vibrational speed (the same temperature), the reaction stops.

These vibrational collisions don't just happen from material-to-material. It happens internally too. The hotter something is, the more violent its internal vibration, which of course causes its own atoms to smash into each other too. That is why heat destroys many materials. For instance, melting a metal like iron is simply the act of bringing it to a temperature where the vibrations are so violent that the inter-molecular bonds of the iron finally break apart its own crystal lattice and it dissolves and becomes a liquid instead. Sure, we might think that things like iron are "solid" materials, but many people will probably be surprised to hear that you can even bring something as solid as iron to temperatures where it's melting (1535*C), and finally actually boiling (2750*C).

That is why heated pulls are better. The heat-vibrations break apart the inter-molecular bonds of the DMT molecules, thus dissolving the big and heavy crystal lattices (structures), and allowing the individual DMT molecules to bond to the solvent instead. As long as the heat is maintained, the particles will stay dissolved. The DMT molecules will either stay bonded to solvent molecules, or they'll stay "vibrating" and free-flowing in the solvent. But as soon as the temperature drops, the super-saturated ( meaning "more saturated than normally possible at room temperature" ) solvent will slow down its internal vibrations, thus allowing the DMT molecules to form undisturbed crystal lattices again (which will no longer be ripped apart by heat-vibrations), and they then become heavier and heavier until they begin dropping out of the solvent. We therefore need to maintain the solvent's heat of a heated pull until the pull is done.

And that brings us to a very related side-note, where it's time to clear up a very common mistake: If you put hot solvent into cold water, you are actually doing a totally cold pull, since the water will rapidly cool down the solvent within seconds and return it to room temperature. The cold water and cold solvent will not be able to heat up the DMT crystals and won't break them apart; so putting hot solvent in cold water is a totally pointless idea and is the same as a cold pull. To get a real hot pull, you must have both hot water and hot solvent, so that the non-polar solvent maintains its heat and the DMT crystals stay dissolved in it.


Onto the topic of freeze precipitation, and why colder solvent can no longer "carry" as much DMT:

When the temperature drops, the vibrations slow down and the DMT molecules have a chance to re-join each other to form crystals again, without constantly being ripped apart by heat-energy anymore. When those crystals become big enough, they become too heavy and they sink out of the solvent. That is how you freeze-precipitate.

If you put solvent straight into the freezer, you immediately remove the heat-energy and cause the "heat-dancing" molecules to calm down and you slow down their vibrations almost instantly. This of course means that they are now free to re-join each other and build new crystals without being constantly broken-apart by heat-energy. But, when their vibrations are extremely slow, they will have much fewer chances to dance around and travel throughout the solvent to bump into each other and form crystals. So when you go straight to freezer, you need about 48 hours for most of them to have a chance to bump into each other. You will also get much smaller crystals (mostly sediment at the bottom of the jar), since the molecules will only bond to their closest neighbors and won't have a chance to "dance all around the jar" to meet bigger crystals and join them.

If you instead slowly cool it; first to room temperature, then to the refrigerator, and finally the freezer, then you'll gradually slow down the molecular vibrations. The heat-energy will calm down enough to stop ripping-apart the crystal lattices (it will stop re-dissolving the DMT crystals into individual molecules), but will still be hot enough to provide enough energy to make the molecules dance wildly. And when they dance; they travel around in the solvent and meet each other and form bigger crystals in less time.

People who are going straight-to-freezer need to wait for the whole 48 hours. People who are gradually cooling need to wait for around 12-15 hours.

If you gradually cool the solution, you don't actually need to monitor your times. It's fine to keep it at room temperature for as long as you want, and the refrigerator for as long as you want, and the freezer for as long as you want. The principle is the same, and there's even a benefit to waiting a bit longer. So people doing gradual cooling should probably spend 1-2 hours at room temperature**, about 2-3 in the refrigerator, and the rest of the time in the freezer. Remember: The slower you cool it, the bigger the crystals. And there's no such thing as "too slow". In lab settings, things can be cooled even more precisely and will sometimes be allowed to cool one degree at a time, over a long period of time.

** About the room temperature step: If you did a cold pull, you should skip the room-temperature step. The reason is simple: Hot solvent is supersaturated thanks to the heat, and when it's allowed to cool to room temperature the carrying-capacity decreases and it becomes even more supersaturated. But cold solvent was already at room-temperature when you pulled, and will therefore not become supersaturated by sitting at room temperature. The only way to get cold solvent to become supersaturated at room temperature is to pre-evaporate some of it. Cold pulls are therefore never recommended, unless you also have access to vacuum distillation to evaporate and supersaturate the solvent without losing any of the solvent, or if you simply don't care about evaporating a large amount of your solvent into the air and losing it forever. People using Naphtha and doing cold pulls usually evaporate some of it, since Naphtha is so cheap that it doesn't matter. But people using Heptane know how expensive that is, and should use hot pulls instead, so that they don't have to evaporate anything.


Here are some more tips that help crystallization:

* Supersaturating the solvent via heated pulls and/or pre-evaporation will ensure that you have lots of DMT molecules in as little solvent as possible. This maximizes the chances of heat-dancing DMT molecules randomly bumping into each other and forming crystals. To help understand this; imagine that you and your brother are in two random places in America. The continent itself is "solvent". The chances of you two finding each other on that vast landmass are extremely small, since there's so much "solvent". So, with too much solvent you won't get any freeze precipitation. But, if you and your brother instead went into the same Supermarket building, meaning a "smaller amount of solvent", then the chances of you two finding each other in the same supermarket is very high. And, if you two went into the same room of a building, meaning a "very very super-saturated, small amount of solvent", then you will pretty much instantly find each other. This is how solvents work and it's the reason why hot pulls are super useful for achieving supersaturation. With hot pulls, less solvent is capable of holding more DMT, thus allowing you to just use a tiny amount of solvent for your pulls, and therefore you won't need to pre-evaporate anything, since the liquid volume will already be tiny.

* If you drop in one or more pre-made DMT crystals from a previous extraction, then you will seed the reaction. This is called a "seed crystal" and its size will attract molecules from the solution, thus growing a big crystal. Just make sure that your solvent has cooled a little bit closer to room-temperature before you drop them in, otherwise the heat-energy will just rip them apart and dissolve them too.

* Some people move the jar back and forth between the freezer and refrigerator every 30 minutes or so. It's a bit crazy and I don't recommend it since it provides almost no benefit. Their idea is that the liquid cools down a bit in the freezer (which might be at -18*C), then heats up a bit again in the refrigerator (which might be at +1.6*C). This constant cycling means that the solvent will spend a lot of time at temperatures between the freezer and refrigerator values, which helps crystallization a tiny bit. But it doesn't help as much as you might believe; because the re-heating process in the fridge is very slow and won't really cause much difference, and because the fridge is already just around +1.6*C which itself isn't very much at all (and will only cause a minor increase in heat-dancing). If you want a hassle-free method of letting the molecules dance, then don't waste your time juggling the bottle between fridge and freezer like this. Instead, just leave it longer in the room and the fridge before putting it in the final freezer. The times I listed earlier are a good starting point.

hah* lovit. "you're both right".
Youcan be whoever r whatever you want, a chemist, a scientist, a lawyer, etc. here, on the DMTNnnexusss.