Confused about crystallization / recrystallization for STB

[frinj]

A fictional character I'm writing about said the following:

I have read many STB tek's, maybe too many, and there is one part that keeps confusing me. I'm probably being really dense, but if anyone can clear this up, I'd appreciate it.

Some background: last night I began my first STB extraction, starting with a low amount of product. I added 20g of MHRB to a solution of 20g lye / 300 mL water and let it sit in warm water for an hour (with periodic agitation), then I added 20mL naptha, let it sit in warm water for another hour (again with periodic agitation), then I attempted to syphon off the naptha layer (as much as I could cleanly syphon), and I added 20 mL more naptha, let it sit overnight and then syphoned off what I could from the naptha layer, added 20mL more naptha, and when I get home from work, I plan to syphon off what I can from the current naptha layer and repeat a few more times.

I think the above is all fine. But I'm confused about what I should be doing with the syphoned naptha. I think some tek's I read had the pulled naptha going straight to the freezer, followed by a filtering to separate crystals from naptha, followed by letting the crystals dry. Other tek's or threads talked about letting the naptha evaporate before freezing (or even as an alternative to any freezing(?)).

I realized last night I had never really nailed down what my approach would be, so I plan on trying a couple alterantives:

FIRST PULL:
I wound up putting the first pull (last night, about 6mL) into a glass jar and putting it straight into the freezer. When I get home from work tonight, it'll be at the 24 hour mark, and I plan to take it out, pour it through a coffee filter to separate the naptha from crystals, then let the crystals dry some more so any residual naptha evaporates off. At that stage, I think I'm done.

SECOND PULL:
I put my second pull (this morning, about 5mL) into a shallow glass dish set in front of an open window to let it evaporate while I'm at work. When I get home tonight, it'll have been evaporating for about 13 hours. I have no idea whether I'll come home to find all the naptha evaporated or not. If I come home and find any liquid still on the dish, I plan to put the dish in the freezer then follow the same process outlined above (wait 24 hours, filter off the liquid, let the crystals dry). If I come home and find no liquid on the dish (meaning all the naptha evaporated while I was at work), it's my understanding that what is left is the dmt crystals and again I am done.

My confusion is that, having read various tek's and threads some talking about evaporation, some talking about freezing, and some talking about both, that I'm not completely confident in my plans for the first and second pull, outlined above. If anyone sees any obvious flaws in my understanding of extracting the crystals from the naptha, I'd appreciate hearing about them.

Also, in some tek's and threads, I read about further steps involving washing and/or recrystalization, but then I also have read people saying these not necessary. I'm not sure why further steps would be needed. I mean, isn't the whole point of the naptha separation that the naptha will NOT suck in any lye or other noxious chemicals, but will ONLY suck in the dmt? So if I did clean pulls of the naptha layer, how could I have gotten any lye or other noxious chemicals in there? And then, as I understand it, the naptha will all either be filtered or evaporated away and so long as I am left with dry crystals, that means the naptha is all gone (since the naptha will never be a solid in this process).

I mean, I understand if I get some funky colored stuff left over on my evaporation dish or freezer jar, that I may need to worry that I have unknowingly pulled in something unwanted and might need to think about cleaning / recrystalization. But if both pulls lead to whitish crystals, is there really any need to do further steps to purify the crystals?

Also, I guess I'm unsure just what the "optimal" way to handle the naptha pulls are in the particular STB tek. Straight to freezer? Evaporate instead of using a freezer? Evaporate until a certain percentage of the naptha evaporates and then freeze? Is one way any better than another? Does my choice of which of these to follow affect my yield?

I'm also wondering if, by doing an extraction on such a small quantity, there is anything special I should know about. I mean, 5-6mL of naptha is not a lot, and I'd imagine it will evaporate pretty fast, so maybe that is a better way to go with such small pulls? Are there any special problems I might encounter because I'm doing such a small extraction? (I already had the problem that my naptha layer was superthin, making it hard to syphon off much clean naptha, with the result that I was only able to pull about 1/3 of the naptha I had added, but I wonder if there are other "small extraction" problems I should know about.)

Anyway, given that my naptha pulls have been relatively small (as a percentage of the naptha added) it would not surprise me if my total yield from these first two pulls is somewhere around under 50mg each, maybe under 30mg each. I'll just be happy if I get any recognizable quantity, and I will use a new container this evening with a super narrow neck that I think will allow me to pull more naptha for my 3rd and 4th pulls for tonight.

Sorry if I've rambled. Any advice / thoughts appreciated.

Frinj

 

[ragabr]

RE: washing and re-x, if you feel very certain that you have not gotten any basified solution along with the naptha, then do not bother. If your bioassays seem unusually harsh, then go ahead and clean. SWIM always does a quick sodium carbonate wash, since it's so easy and quick, but not a big deal.

Her preference goes with the freeze precipitation, as she can then go on to re-use her naptha. Evaporating will give you larger crystals, but though beautiful, she doesn't concern herself much with that.

 

[endlessness]

your understanding is pretty much correct.. before answering some questions, a note: you say you added the naphtha to the mimosa, let it stand and then syphon off.. was there no mixing? Because you have to not only put the naphtha there but mix it, let it stand, mix a bit more, let it stand again, and do this a few times, so that the naphtha get in contact with as much dmt in the mimosa mix as possible.


As for final method of crystal retrieval, each one has its advantages and disadvantages but they should all work. Freeze precipitation normally yields purer crystals, because any plant fats that may be dissolved in the naphtha will continue for the most part dissolved in it, while the dmt will crash out. Alternatively, evaporating will mean whatever the naphtha picked up, including plant oils, will be together with your dmt. So its likely your evaporated dmt will be more oily/yellow. Also there is the added fact that evaporating, specially with fan and/or heat might create some dmt n-oxide, that is still psychoactive but its a goo so it wont crystalize (or if its small quantities it might just make your dmt a bit more yellow/oily). The other disadvantage of evaporating is that its wasteful. The advantage I guess is no need for freezer, just let it stand there... When I used to extract with naphtha I preffered freeze precipitating, because of purity but also because of being able to reuse the naphtha

The idea why people pre-evaporate some naphtha before sticking in the freezer is that, for freeze precipitation to work, its better the more saturated your naphtha is, otherwise some dmt might not precipitate.. let me quote myself on an explanation I gave about this on another thread, when asked "does it matter how saturated the naphtha is for freeze precipitation":

Yes sure it matters how saturated. The whole point is that naphtha should be as saturated as possible so that once the temperature goes down, naphtha will hold even less DMT so most will precipitate. If there's too much naphtha, even at freeze temperatures it might still hold most of your DMT.

As an imaginary example (not real numbers, just to illustrate the point), lets say 50ml naphtha holds 1g dmt at room temperature, and at freeze temperature 50ml of naphtha only holds 100mg DMT. So if you had 50 ml saturated naphtha and you put it in the freezer, 90% of your DMT will precipitate. Now if you instead had that 1g of dmt dissolved in, say, 200ml naphtha, when you put it in the freezer, even in those temperatures, if we take these numbers im using, then at least 400mg of dmt wont crash out, meaning you are 40% of your dmt is not crashing out.

So yes, as saturated as possible is better. There's two things you can do now: 1- pre-evap a significant amount of the naphtha before sticking in the freezer
or 2- Stick it in the freezer as-is, and after a day or so of precipitation, retrieve any crystals that might have precipitated and reuse the naphtha for more pulls (meaning the unprecipitated dmt wont be lost, it will be there for next pull), or if its your last pull, evap it till the end to retrieve the rest of your dmt.

so yeah, same is valid for you. you can test the naphtha saturation by blowing on it. If it gets cloudy, you can stick in the freezer.. if not, then better pre-evap a bit.


as for the wash and whether its ok to smoke without it, yeah if you made good separation you shouldnt have any lye/mimosa mix so its ok to smoke as is...

you are extracting a very small amount, so first lets hope it goes good.. if it does and you feel like extracting some more eventually, I suggest doing a test and making a wash with half of a pull, and not washing the other half, and then freezing them and trying them separately, to see for yourself if you think washing is necessary

btw, maybe this thread is also of some help to you, specially the part "your spice is ok to smoke when....", because it deals with your question whether the naphtha should be all gone when evapping and so on.

oh and lastly, about how to retrieve the crystals from freeze precipitation, some people have the famous 'melting crystals' problem once the container is out of the freezer, so I suggest you look into this way of retrieving the crystals because it helps preventing the problem:

 

[frinj]

Thanks a lot!

Oh, and I did shake the sludge up after adding the naptha.

I have a certain bottle of liquor with a VERY thin neck I was going to empty out and use tonight so that my third naptha pull will (hopefully) be larger than the first two. Is there any danger putting the lye/naptha sludge in a bottle that previously contained hard liquor? Obviously, I will rinse it out thoroughly, but given how thin the neck of the bottle is, I cannot get a brush inside it and I want to know if there is any risk of a big, bad chemical reaction if some trace amount of alcohol remains in the bottle when I add the lye/naptha sludge.

I also read that one risk of using an evaporation-only crystalization is impurities in the solvent. I am using VM&P Naptha, which I thought I read was 100% naptha. Does that mean this is not a risk when using this particular solvent, or does even VM&P contain trace additives that could remain post-evaporation to contaminate the dmt?

Also, maybe I should know this, but does the volume of naptha (as distinct from the saturation level) affect how quickly the dmt crashes out during freeze-precipation? Before I left for work this morning, I checked my jar from the first pull that I'd put in the freezer, and the bottom of the jar seemed to have a good amount (relatively speaking) of visible crystals even though it had only been in there about 8-10 hours, and I wondered if everything goes faster when you work with such small amounts (only about 6mL of naptha in the jar).

It's kind of the same idea that a shallow dish of water will freeze faster than a deep dish of water. Thus, a smaller amount of naptha should fully cool down to the freezer temperature and reach maximum crash out faster than a larger amount of naptha (even if the saturation level is the same in each). I'm a newbie at this, but my completely speculative theory is that, if this is true, it might make sense to divide one's naptha pull between numerous jars / containers / dishes to go into the freezer (assuming one has the room) to cut down on the time needed for the freeze-precipitation stage.

 

[physics envy]

Thanks for the question frinj - SWIM is also trying to figure out the easiest method for himself and appreciates the tips given above. SWIM has especially had the melting crystals issue...blech.

SWIM is now testing out using a big flat baking glass covered with seran wrap in the freezer as using jars has been a pain. Hopefully this won't smell up the freezer! He has had trouble getting the crystals out after freezing. Perhaps he hasn't found the right jars to use - he found some wide-mouthed quart jars at Walmart but he can't really get his hand and a blade or scraper in the jar. Maybe he was overlooking something, however.

If SWIM may, he would like to add a question to this thread that seems pertinent: what is a safe and (relatively) quick method to pre-evap? SWIM has read of some nice setups using fans and filters to block bugs, etc., but could one use a double-boiler setup to keep the pulled liquid hot, along with some airflow? Other similar solutions?

 

[frinj]

My fictional story writing continues. Here is my main character's latest adventure, told in first person:

I took the first pull from the freezer last night (after about 24 hours), put the jar upside down over a coffee filter in a funnel over a larger jar and then stuck that whole thing back in the freezer for a few hours, to let as much naptha as possible drain while trying to avoid any "melting" effect. After a few hours, the top (upside) jar was scraped as well as I could -- it is a small jar and I could only find a metal spoon to use, and whatever was left was still somewhat moist / oily. Wound up scraping a bit of yellowy / waxy stuff onto a flat glass baking dish. I looked in the coffee filter and it has some dry and very white crystals that came off easy and also went into the baking dish. They came off easily enough that I wonder if I should have put EVERYTHING I scraped out -- all the yellow, waxy stuff -- onto a coffee filter to sit in the freezer for a few hours in the hopes it would dry into similar white crystals. But I didn't. Instead, I put the baking dish by a window to let evaporation do whatever it could do overnight. I still could smell naptha from the yellow waxy stuff I'd scraped onto the baking dish. It sat by the window overnight. This morning -- no naptha smell, but the yellow waxy stuff is still yellow and waxy (or maybe oily is a better word for it). Anyway, I think there is maybe 20mg of material on this baking dish (this was a very small pull from a very small reaction). I do think now that some kind of cleaning / washing / recrystalization would be nice.

The second pull, which was put directly into a shallow glass dish by the window for about 12 hours, appeared to be empty when I got home. On closer examination, it seems there is a sticky/oily clear layer on the plate. I put this in the freezer overnight to see if that would promote crystalization of whatever is left, but I'm kind of pessimistic about this particular pull. In the morning, the bottom of the plate was a bit cloudier. Maybe if a took a razor blade and tried scraping whatever that cloudy layer is, I might find there is something salvageable, but I did not have time, so I set the plate aside (not in the freezer, just at room temp, and covered) to deal with tonight.

Also a friend brought over a lab-quality separatory funnel. It was kind of tricky to use without a support stand or other lab apparatus. Anyawy, I poured off most of the naptha layer on my sludge, along with a fair amount of sludge, into the separatory funnel, let it settle for about 30 minutes, then funneled the sludge layer back into the mother bottle. There's a bit of a learning curve with a separatory funnel, but I pulled more naptha than either of the first two pulls. Given the yellow / waxy product I produced without cleaning, I did two sodium carbonate washes, a cold water wash and a dried epsom salt wash. All went smoothly. Here, again, I came up with the conundrum -- whether to do a partial evap, or go straight to freezer. As it was late and I am lazy, I tossed the resulting solvent into the freezer. I am using a small, deep glass bowl (more of a dipping sauce holder) this time, which should have easier access for scraping crystals than a jar. I feel more confident about getting some nice clean crystals from this pull, maybe enough for one hit (?)

The relatively small amount of naptha I'm working with is still making everything harder. I have been adding 20mL of clean naptha per pull. Considering I've done 3 pulls, and all pulled less than 10mL of naptha, I should have over 30mL of naptha residual in the jar, but I do not really see that. I'm not sure if any portion of the naptha stays in tye lye/sludge layer, or evaporates or anything. I have not measured my naptha pulls, so maybe I'm underestimating how much I have pulled. Oh, well, the point is that I wanted to have an easier time with my 4th pull, so I added an unmeasured quantity of fresh naptha to the sludge which I estimated to be around 30mL. I also added the naptha left from my filtering of the first pull. I rolled the mother bottle around and around. I figure adding extra naptha means I should probably do a partial evap before freeze-precipitation on the 4th pull, but my thinking is that it'll be worth it to not have to deal with such small quantities.

In retrospect, here's what I mainly learned:

1. You may be tempted to do a very small extraction your first time to avoid wasting product if you screw something up, however, that may just make it harder and make it more likely you WILL screw something up. If I had it to do over again, I'd do at least 50g of MHRB, probably 100g.

2. Once you have a good system set up for funneling / decanting / whatever, the washing steps are a piece of cake with sodium carbonate and epsom salt. (Followed Whatcha's tek for this, and pretty much the whole thing.)

Well, anyway, I'm not done yet.

 

[HyperD]

1. You may be tempted to do a very small extraction your first time to avoid wasting product if you screw something up, however, that may just make it harder and make it more likely you WILL screw something up. If I had it to do over again, I'd do at least 50g of MHRB, probably 100g.

.

Yes indeed!
I would go for at least 150-250 mg mimosa like Frinj says,otherwise it makies you "greedy" when separate small amounts so you pushing the limit and can get "black stuff" in the hepthan

 

[frinj]

More about my fictional character, written from his first person perspective:

An update on my first STB dmt extraction (or any extraction, for that matter) or "what I did last night."

RESULTS OF FIRST AND SECOND PULLS.
The results of the first and second pulls have been sitting in glass dishes at room temp the last 24 hours. The first pull results consists of a yellow, waxy smudge and a few white specks. The second pull results (which I evaporated for 24 hours before putting into the freezer) consists of an oily clear residue on a plate. Neither pull went through any kind of wash at any stage. Disgusted, I gave up on both and rinsed off the dishes.

RESULTS OF THIRD PULL
My third pull was taken from the freezer, a glass bowl with some naptha and some nice white crystals in the bottom. I poured off the naptha into a coffee filter put in a plastic funnel sitting in a small jar, then put the same coffee filter flat on a plate with the bowl of crystals turned upside down on it, and put that in the refrigerator. My thinking was to let gravity pull at least some residual naptha run off of the crystals in an environment that was cool enough to avoid risk of re-evaporation into the naptha. I guess the freezer might have been a safer bet, but I had more room in the fridge. I let that sit for a few hours.

Just before bed, I took it out, looked at the filter and was surprised to see no crystals on it at all. I mean, this was the filter I'd used to strain the naptha when I first took it out of the freezer, and I guess I'd assumed some crystals always get carried off as you pour off the naptha. However, all I can imagine is that all the freeze-precipated crystals were securely fastened to the glass dish so this did not happen. Anyway, filter was discarded, glass bowl -- now upright -- was set in front of a window covered by a paper towel to allow for further drying. I'm guessing there may be 30mg of crystals there, which may seem tiny, but was coming from a third pull from a very small extract. Anyway, I could be wrong about quantity, may be able to weigh it tonight if it has dried enough. I have no plans to recrystalize, since I did the pre-freezer washes of the solvent.

FOURTH PULL
I took my sludge from the mother bottle and put half in my separatory funnel (all that would fit) and let it settle. after about 15 minutes, so I separated out the sludge layer from the solvent layer, poured the solvent into a jar. I then added the other half of my sludge into the separatory funnel, waited 15 minutes, then repeated this process. I realize it might save time if I could pour off the naptha layer with some sludge and then put that into the separatory funnel, and I'll probably do that with any larger extraction. Putting all of the sludge into a separatory funnel a couple hundred mg's at a time, could take quite a while for larger extractions.

I did two sodium carbonate washes and one water wash on the solvent per Whatcha's tek, but then forgot to do the epsom salt wash (and the epsom salt was already warmed in the microwave). I was using the separatory funnel for these washes, and I think that meant I got little residual water in my solvent, if any. The washed solvent was put into a glass bowl and put into the freezer (with a lid). I'll deal with it further tonight, or maybe tomorrow morning.

FIFTH PULL
I put the remaining sludge into an hpde 1/2 gallon milk jug. It had been in a glass tequila bottle for the last 2 days, but I recently read some one warning that very base solutions can etch glass and cause it to shatter, and so I did not want to risk that. There was 1/2 inch of solid-ish sludge in the bottom of the bottle that would not pour out. I am thinking this means I did not have enough lye-water solution(?) for the amount of MHRB. I figured some fresh lye-water solution would be the trick to get it out, and would also help my next pull. I added 5g lye to 100mL water (slowly with stirring), then poured that into the glass bottle, it broke up the remaining sludge material nicely, then that was all poured into the milk judge with the other sludge. The jug was put into a sink filled with hot water for about an hour, shaken periodically. Then I added both the naptha I'd filtered off of my 3rd pull (maybe 10-15mL) and another 15-20mL of fresh naptha to the milk jug. I had tried to somewhat warm the naptha first by putting it into a small jar sitting in a larger bowl of hot water. After the naptha was added, I rolled the milk jug around rather than shaking it, to avoid emulsification (whatever that is) then put the jug back into the hot water in the sink. I'll likely pull this tonight, and it may be my last pull.

OVERVIEW
I'm excited to see the 3rd pull results tonight. If the spice has dried completely, and there is enough there, I might be able to try visiting hyperspace tonight. If there is not enough there, I still feel pretty confident in my 4th and 5th pulls. The real difference has been the separatory funnel because trying to cleanly siphon off a 20mL layer of naptha was ridiculously hard. If I'd started with a larger volume of everything, the separatory funnel probably would not have been that critical.

Oh, I did notice that I sniffed a lot of naptha last night. Since I was using various jars, I kept picking up a jar and sniffing it to tell if it was naptha before using it. I do not know just how unhealthy this is, but I was feeling kind of queasy when I went to bed, and I think from now on I want to figure out a better system for keeping track of where my naptha is so I don't have to sniff it to find out.

 

[frinj]

Update:

THIRD PULL
On Friday night, I scraped of the crystals from my third pull, weighed about 45mg. This seemed about right, considering this is a third pull from an original 20g of MHRB.

FOURTH PULL
Without going any details, I got about 5mg of crystals from the 4th pull, which was disappointing. I'm wondering if the pH of my sludge has gotten out of whack, but I have no wide range pH papers to test it. Alternatively, I wonder if the sludge is simply out of spice at this point, meaning either the MHRB was weak to begin with, or I wasted quite a bit with my inefficiency during the first couple pulls. I also admit my choice of glassware was not too good. While doing washes, I would up putting the solvent in jars to which I had no matching lid, with the result that I tried a makeshift lid and solvent leaked out and got on my hands. So some spice was definitely lost in that process. Another thought occurred to me that perhaps my freezer is not cold enough.

FIFTH PULL
Friday night, I made a fifth pull of solvent, using the separatory funnel. When I blew on it, I saw no cloudiness, which I understand is a sign that the naptha is not saturated and I should use evaporation. However, I was lazy and put the jar into the freezer to see what would happen. That was Friday night. As of Sunday night, still no crystallization. Given the poor results of my 4th pull, it is possible there is simply no spice left in the sludge. It is also possible the lack of saturation is inhibiting freeze precipitation. I am also wondering if my freezer is not cold enough.

SIXTH PULL
Not wanting to give up on the sludge (and since I may want to save it and ultimately try a jungle spice extract), I added more naptha to the sludge on Friday night and set the jug aside. I have not touched it since then. This will definitely be my final spice pull, though I may try a jungle spice pull later. I'm not sure if I'll pull the solvent tonight or give it a couple more days.

To recap, I discarded the minimal results of my 1st pull, saw no results from my 2nd pull, got 45mg from my 3rd pull, got 5mg from my fourth pull, and I have not yet seen what the fifth or six pulls will yield.

Frinj

 

[StrangeLoop]

I've found the best method for getting crystals out of jars is to shake the EXTREMELY COLD jars up, then using a rubber spatula, try to knock off as much of the remaining crystals into the naphtha, preferably either still in your freezer or in an ice bath. Give it another shake and then quickly filter the crystals. If done properly, only a minimal amount of spice if any will redissolve and most of it will be in the coffee filter, which can be air dryed in a few minutes.

At first I tried just air drying the jars and scraping, which resulted in yellow waxy DMT even though the crystals were white on the glass. I think a fair amount of solvent gets trapped between the crystals and the glass and never really dries out very well, which is why I've taken to this new method.

And you definitely need to be working with larger amounts of bark. I worked with 100g bark and ~50mL pulls and the organic layer is still very very small compared to the mimosa goop making it hard to separate. Alternatively you can still do small scale extractions but you need specific equipment for separation such as a centrifuge tube and filter tip pipette.

 

[physics envy]

SWIM is pretty new to extractions, but he found the q21q21 tek using lime & vinegar to be MUCH easier for siphoning off the solvent layer than his previous attempts using lye teks. The mimosa soup was much thicker, and SWIM was able to VERY VERY EASILY simply pour off the solvent without getting any of the soup. You can even hold the soup back with your hand if you like (SWIM used a wooden spoon but basically just poured the naphtha off).

You are right though...larger batches make the extraction easier with the lye methods. SWIM, in his inexperience, hated the turkey-baster and had problems pulling in mimosa soup almost every time. Or you can just use extra naphtha...SWIM doesn't suppose that could *hurt* anything.

 

[StrangeLoop]

Extra naphtha wouldn't hurt, but some would have to be evaporated off before freeze precipitation.

The turkey baster is so much more annoying than I imagined, for some reason I just thought of it as an oversized pipette but the physics of it just aren't the same. :lol: I usually just siphon off all of it from my jug, including some goop, into a clear plastic glass, and then siphon again with a smaller amount of goop into a graduated cylinder. Then I rinse the baster with fresh naphtha, and siphon out of the graduated cylinder into a jar. With a tall and skinny container like that it's very easy to get 99% of the solvent.

I may have to try the lime and vinegar tek but I have everything I need for Noman's and it's worked just fine for me so far.