Freeze Precipitation 25 Hours In - Looking for Advice!

[SweetGreg]

Hello fellow Nexus members,

I am a first time poster here at the nexus and a first time extractor as well; however, I have been an active viewer of the nexus forums for a year or so now. Just two days ago I started my first extraction of spice from Mimosa tenuiflora rootbark powder provided by the reputable CS supplier.

The tek I followed was the marvelously simple and convenient (yet I am told effective) "Whatcha's Easy MHRB STB Extraction Tek." I followed the guide mostly to the T, using 2 pounds of bark powder and 2 milk jugs. The only variations I made were adding some more water to make my mixture slightly less sludgy.

Mid process, during my naphtha pulls I encountered the dark brown/red naphtha curse reportedly often seen in STB and/or pre-powdered barks extractions, both of which I utilized. After completing 8, 400ml naphtha pulls my collection jug was a dark brown and red still. I proceeded to perform a total of 4 sodium carbonate washes to finally make the color a deep yellow or orange. No residual lye or floaters were seen by this point either.


** One thing to note and a question I had was my 4th wash was still colored, I proceeded to do an epsom salt dry however out of fear of possible yield loss from repeated washes. **Should I have continued to sodium carbonate wash until the wash water came out clear?** **Will a sodium carbonate solution at pH 10-11 even sap spice from the naphtha?**


Finally, my naphtha jug has now been in the freezer for 26 hours and am seeing a considerable amount of solidified precipitate at the bottom of my jug with more forming higher up in the naphtha and falling slowly to the bottom. I am assuming the attached photos of my jug contain spice (the layer at the bottom and not some weird gunk).

**My main question I guess is how much longer should I keep my jug in the freezer. I am anxious to remove it but all the same paranoid that the precipitate wont be spice and just some sludge lol. Also, if anyone could eyeball that and have a random ballpark guess of the yield in there? It couldn't have been that easy.**

 

[Ljosalfar]

Looks great!
You can decant (some folks filter, but why bother? see below), dry what has crashed out so far (cool air and a fan), and assess - you'll probably have a nice pile of canary spice.Re-crystallization with a small volume of heptane is nice, thus eliminating some of the oil/fat/wax impurities. Re-x is not essential but does give a purer product. Try 1g in a shot glass to get the feel for this simple step.
Return the decanted solvent to the freezer, and check to ensure it is at its coldest setting.
A bit more should crash out in the next few days. No way to know the yield until it is weighed.
Don't throw anything away.
Best,
L

 

[MelCat]

I'd probably evap some of the excess naptha before returning to the freezer. That's quite a bit of solvent you have there.

Once you've evap'd the naptha down to around 200-300ml, put it back in there and you should have a blizzard within 24 hours.

 

[SweetGreg]

I managed to find some errands to run today to stall my impatient nature and let it sit in the freezer longer. I plan to remove and decant the liquid into a new jug later tonight after around 32 hours, and then scrape all the spice and air/cool low setting fan dry like Lj suggested above, thank you by the way!

And Melodic, once I evap the decanted liquid down to said 200-300ml you think there will still be a lot more to pull out of it than whats already shown in the photos? I know that the more solvent there is, the harder it is for the spice to precipitate out, that's basic chemistry....but I currently have 3000-3200ml and quite a bit of spice has crashed out already, I'm hoping/guessing this must mean that jug is fairly saturated then ?

And thank you both, everyone here is a lot of help. Good advice all around!

 

[MelCat]

Definitely.

If you've got 3000 ml and you're precipitating goodies already, then once you evap it down a bit it's really gonna snow.

I didn't realize that you had 3000ml.. Maybe just evap it down to 1000ml, freeze and then evap it down to 200ml and try again.

Looks like you're on the right track though!

 

[Carrierwave]

you win the award for using more solvent than anyone probably ever has.

Evaporate that down to 1/10th that volume and freeze it again. Also possible you have frozen water at the bottom of your jug. DMT forms crystals, the kind you could never ever mistake for ice. Keep that in mind.

 

[Ljosalfar]

Personally I avoid evap - I like to recycle the solvent and avoid putting it into the atmosphere. And be sure if you do evap, do it outside or with plenty of ventilation.
3 liters is a lot - I would divide the decanted solvent into 3 volumes in glass and put into the freezer for a week - spice will precipitate and may form large crystal 'flowers' over this extended freeze. It is true that precip/crystallization is slower in less saturated solutions, but with a week of patience a few really nice raisin-sized 'flowers' were an awesome windfall. Again, the colder the better. Glass jars are easier/cleaner to recover goodies from, IMHO, although HDPE jugs are a trusted classic!
A fun accelerator is dry ice - check out the Ice Cream Tek!
Best of luck, let us know,
L

 

[Ljosalfar]

DMT forms crystals, the kind you could never ever mistake for ice.

Yes, best to avoid all water - sounds like the OP did dry with an epsom salt wash. Occasionally a bit of H2o will sneak in and then one needs some patience to let it evap, and then usually a re-x is in order.
DMT may be obviously crystalline, but frequently it's a hard-boiled egg yolk consistency and color due to impurities, especially with STB extractions. This is what the photos appear to show - that delightful slush. Canary spice! Again, re-x will bring out the shards and lose the oils, if this is what you're after.

 

[cyberdream]

looks nice , i would evap and put in freezer again good luck

 

[SweetGreg]

Hello everyone. I am back bearing bad news about my extraction. Upon removal of the jug and decanting the solvent into three separate containers I was left with a nice amount of orange/brown-ish spice. Solid, powdery, not fine crystals, but I knew it was from fats and oils probably. I was pissed my naphtha pulled so much stuff that not even 4 sodium carb washes of fair volume could fix it. I should have done 6 or 7 looking back.....

I was left with what these photos show here, I believe it to be the mystery brown active dmt gunk where the dmt has dissolved or at least collapsed and settled into plant fats and oils that melt at room temperature?

I am in a bind and very scared I have fucked this up. There was a fair bit of powder, I'd guess minimum 5-6 grams but I never got a chance to weigh it since it melted as I evaporated the remaining naphtha with a cool, distant fan. Also, precipitate crystals show up occasionally in the container on sides of walls and redissolve when in contact with gunk.

My questions begin in WHAT DO I DO? Lol. I have read about mini A/B extractions that may fix my problem, but the guides I found posted on forums seemed rather vague with vague figures and measurements. If so be it I will do the A/B hands down if it will get me my clean spice out of that gunk; however, I read somewhere that people were discovering that 100% acetone was an effective dmt freebase solvent and would not hold much if any of the plant fats/fats/tannins. I also read that you need little and it evaporates quickly. Is this methodology totally flawed or does anyone think it may have merit? It is my understanding acetone will also evap very quickly leaving behind pretty spice.

If that solution does not work would a heptane re-x be possible with the gunk? Every guide I read for re-x or fixing dirty spice with acetone or heptane, etc gives figures for powder...but I have gunk....:/ its not even a solid.

I just feel like I am in a bind and am wondering if I will be able to get my precious spice back. I remember the gallon jug even had the pungent familiar spicy smell. Also, do you think that much gunk means that my spice solids were more oil/fat than spice itself?

Help much appreciated, thank you!

 

[Ljosalfar]

All is not lost! - I speculate that water is your problem, due to so many carbonate washes. My understanding is that carbonate washes are for gently eliminating traces of lye solution, NOT for eliminating the fat/oil/wax. The fat/oil/wax is always present in an STB, and can be a pleasant (!!!) smoke - not necessarily bad.
Have some patience, and dry the 'gunk' out (not with epsom salt, just a fan if you like - if water is indeed present this may take a while), observe any changes.
Then, when you are confident you only have product and no water or remaining solvent in there, dissolve it completely with warm heptane. Do this in a small, clear glass, wide-mouth tumbler or some such. Cover it tightly and place it in the freezer. Your re-x is under way. You will probably see crystals forming in a few hours - darker fats and oils will be clearly visible at the bottom and the glass will be encrusted. Decant and gently dry the glass.
Voila!
Don't throw anything away.
Best,
L

 

[SweetGreg]

Okay, I will have it sitting out in the air partially covered to avoid intake of dust particulates. I currently have to wait on my fan option again; however, I have heard of people who have never been able to successfully solidify the gunk. I feel like there is definitely some stuff left to evaporate so I will wait. If it stays a semi-liquid, think goop will that still be good to put in heptane? Also, would putting it in the freezer with the container open be a good/bad idea?

 

[MelCat]

Also, would putting it in the freezer with the container open be a good/bad idea?

Yeah, that would be a bad idea. It would allow even more water to get into the solution.

You just want to dry it out the best you can and then warm up some heptane (not too hot) and mix the goop as much as possible. I like to mix it a couple of times just to make sure I get all of the pure spice out of the oils. As Ljosalfar said, the oil will go to the bottom of the container. Heptane is a very selective solvent and will only pick up the pure spice.

Decant this new heptane solution into another container and cover the container with saran wrap or aluminum foil and poke a few holes in it. The slower this solvent evaporates, the better your crystals will turn out. Also, don't move or jostle the container while the crystals are growing as it will affect their growth. Leave it sitting for at least a couple of days but longer wouldn't hurt either.

Once your crystals are formed, carefully remove the excess solvent and save it. It's possible that all of the spice didn't crystallize out of it, so you can save it for your next re-x or evap it the rest of the way.

As for the goop that collected at the bottom... You're right, sometimes that won't solidify no matter how long you leave it. When this is the case, I dissolve it in some IPA and infuse it to changa or enhanced leaf. Way easier to handle and looks discreet as well.

Good luck

 

[SweetGreg]

Okay good deal, so keep the gunk that separates out of the heptane? Also, if staying a gunk, it will be rather difficult to measure. How would you suggest determining the amount of warm heptane to use on the gunk?

 

[MelCat]

Okay good deal, so keep the gunk that separates out of the heptane? Also, if staying a gunk, it will be rather difficult to measure. How would you suggest determining the amount of warm heptane to use on the gunk?

Depending on how much spice you have and the container you use, I'd say cover the spice with at least an inch of solvent and mix it up a few times to pull as many alks as possible.

You could even do a few pulls to make sure you get it all but that's your call. It will just take a little longer for the crystals to form and for the solvent to evap. Or evap the pulls separately.

Either way, let us know how it turns out.