Please Help! Evaporate Excess Naptha after Freeze Precipitation?

[musicguy24]

Help!!! This is my first post, I'm kind of a noob at this stuff, but I have loved this forum for a while, you guys are truly a different special community. I've done a ridiculous amount of research on this so if this is a repetitive question, I'm sorry. I tried! I want to make sure this extraction goes well.

SWIM in the middle of their first extraction using Noman's TEK with a Sodium Carbonate wash right before freeze precipitation. They're not really sure how it's going thus far. They can see what appears to be crystals(could be ice) in their jars. After leaving the jars in the freezer for nearly 48 hours they decided to take one out and try to get a little bit of spice out of the jar to test out. When trying to remove from the jar with a spoon the crystal(or ice) melted very quickly within 20 or so seconds of being in the spoon :shock: , my friend said they couldn't tell if it was oily or more water-like. Perhaps their freezer isn't getting cold enough? I told them putting some dry ice in the freezer could help with that, hope that was true. They just started the freezer>fridge>room>fridge>freezer>repeat method, within 30 minutes of going from the freezer to the fridge almost everything had dissolved into the naptha. My question is what could be going wrong with it melting like that? My prediction is the freezer isn't cold enough? OR is it possible that there is too much naptha in the jar for the spice to form well? If so, how could I go about getting some out the most efficient way. Will the freezer>fridge>room>fridge>freezer>repeat method slowly evaporate the naptha? Appreciate your help a ton!

 

[boogerz]

welcome!
here

 

[Vitalstatistix]

how much material did you start off with and how much naptha did you use? Also what material did you use? MHRB, Acacia bark, Acacia phylodes, Phalaris?

I would say without a doubt that what you are seeing in the naptha are ice xtals. Any air with moisture that is inside your sealed freeze precipitation jar will cause some ice to form.

Is the naptha cloudy in appearance when it has been in the freezer for some hours?

If it is not cloudy then it is either very dilute or contains none or very little spice. Try evaporating down your naptha before freezing. I don't have a very cold freezer but it will freeze preipitate spice from naptha. My friends is not as good as mine and his works too. You should evaporate the naptha until it becomes cloudy and then put it in the freezer.

When using a STB tek you really need to give the soup a good amount of time to sit because DMT freebase is not soluble in water it can take quite a bit of time sitting there before the spice comes out and the naptha can access it to take up the freebase which is very soluble in it. If your bark is not powdered very fine i would advise leaving your soup to sit with naptha on it for at least 48 hours. The NaOH will eat away at the celulose holding the cells together making the DMT more accessable to the naptha.

One thing about DMT extractions is that a good extraction takes patience.

I preffer A/B teks more myself. Somehow I find them more rewarding.

 

[musicguy24]

Thanks for your reply and help!
Oh yeah, should have mentioned that he only had 50g of MHRB to start off with.
Just wanted to test out the procedure with a little bit before he did bigger extractions.
Yeah, it's got to be ice.
Yes, the naptha is cloudy when it's been in the freezer for a while.
To evaporate the naptha just leave the jar sitting out sealed? Noob question I'm sure...
Yeah, SWIM is definitely considering trying an A/B tek next time.

 

[Icon]

I don't think much of swapping it between freezer/fridge to remelt and rebuild larger crystals. In my experience, it's made even smaller and less stable crystals. I just pop the dish of naphtha into the freezer for 2-3 days undisturbed. It's very tempting to peak at the progress, but seriously just forget about them for a few days so they can grow without being sloshed around.

The exact same thing happened my first extraction. I was all excited about my white specks that I poured off the naphtha and tried to scoop them up with a spoon. Boy was that a mistake, the glass was still wet and the crystals just smeared around and melted before I could even pile them up. What you should try is pouring off the naphtha and then letting the dish sit still for a few days to dry. Any residual naphtha might try to redissolve your crystals, but after a day the drier glass is much easier to scrape up and the crystals fall from the glass like grains of sand.

I imagine the crystals from a 50g extraction are pretty small though, evaporating the naphtha down to a higher concentration before freezing might help you a lot.

Oh I also suggest a razor blade and a more accessible container for scraping. A spoon in a jar isn't going to give you a very good angle, and will probably just smear the crystals into a dusty powder along the edges of the glass.

 

[musicguy24]

I don't think much of swapping it between freezer/fridge to remelt and rebuild larger crystals. In my experience, it's made even smaller and less stable crystals. I just pop the dish of naphtha into the freezer for 2-3 days undisturbed. It's very tempting to peak at the progress, but seriously just forget about them for a few days so they can grow without being sloshed around.

The exact same thing happened my first extraction. I was all excited about my white specks that I poured off the naphtha and tried to scoop them up with a spoon. Boy was that a mistake, the glass was still wet and the crystals just smeared around and melted before I could even pile them up. What you should try is pouring off the naphtha and then letting the dish sit still for a few days to dry. Any residual naphtha might try to redissolve your crystals, but after a day the drier glass is much easier to scrape up and the crystals fall from the glass like grains of sand.

I imagine the crystals from a 50g extraction are pretty small though, evaporating the naphtha down to a higher concentration before freezing might help you a lot.

Oh I also suggest a razor blade and a more accessible container for scraping. A spoon in a jar isn't going to give you a very good angle, and will probably just smear the crystals into a dusty powder along the edges of the glass.

I'm slightly frustrated because I have been reading about how to do this for days, but I feel like I almost have a good understanding. You seemed to bring up most of the things I'm still unclear about. I'll tell him not to waste his time with all of the moving around of the jars from freezer to fridge and back. I think it's very possible that they've just moved the jars around too much. They definitely didn't leave the jars alone for 2-3 days, that's for sure. Where should the jar be when it's drying? Lid on or off? 3 days ideal drying time? How do you recommend the naptha be evaporated before freezing? Yeah that's a good point about jars too, need to find something square-like...
This is very helpful, appreciate it!

 

[Icon]

Where should the jar be when it's drying? Lid on or off? 3 days ideal drying time? How do you recommend the naptha be evaporated before freezing?

Certainly lid off, so the naphtha can evaporate off of the dish and into the air. If you're evaporating before freezing, set it in a well-ventilated area under a fan or something that will keep the fumes from building up. Simply let it sit lid-off to evaporate 20-50% of your solution.

When you're letting the crystals dry take the lid off and let the dish dry upside down in the freezer for a half hour(to let any drops drip to the rim so you can wipe em off). Then take it out of the freezer and just set it right side up, lid off by a window or whatever to let the remaining residue evaporate. 3 days is probably excessive--I do the smell test, and generally after 2 days I can't smell a whiff of naphtha and I know they're ready to go.

 

[musicguy24]

Where should the jar be when it's drying? Lid on or off? 3 days ideal drying time? How do you recommend the naptha be evaporated before freezing?

Certainly lid off, so the naphtha can evaporate off of the dish and into the air. If you're evaporating before freezing, set it in a well-ventilated area under a fan or something that will keep the fumes from building up. Simply let it sit lid-off to evaporate 20-50% of your solution.

When you're letting the crystals dry take the lid off and let the dish dry upside down in the freezer for a half hour(to let any drops drip to the rim so you can wipe em off). Then take it out of the freezer and just set it right side up, lid off by a window or whatever to let the remaining residue evaporate. 3 days is probably excessive--I do the smell test, and generally after 2 days I can't smell a whiff of naphtha and I know they're ready to go.

Okay cool, I was guessing lid off haha
I've heard of drying in the fridge?(No food in fridge)
You think drying out by a window would be better?
Is it too late to evaporate some naptha after you do freeze precipitation? And then try to re-freeze? I know that's not the ideal method, but if you're in the current circumstances of SWIM...
Thanks for answering my noob questions. You are awesome!!!

 

[Icon]

Okay cool, I was guessing lid off haha
I've heard of drying in the fridge?(No food in fridge)
You think drying out by a window would be better?
Is it too late to evaporate some naptha after you do freeze precipitation? And then try to re-freeze? I know that's not the ideal method, but if you're in the current circumstances of SWIM...
Thanks for answering my noob questions. You are awesome!!!

Well it really doesn't matter where it dries as long as it gets good air-flow. For this reason, by a window or under a fan is what works best for most. Just leave it in an open area and try not to let it collect dust or dirt from the air. (so don't leave it out on your back porch)

Yea that's fine if you want to evaporate down some before re-trying the freeze precipitation. That's called a "re-crystallization" and isn't necessary unless you need to rebuild gooey crystals or make a more pure product. In your case, I'm guessing you have a sticky goo on the bottom of your jar/spoon, so just heat up like a shotglass worth of naphtha(so you don't have to evaporate any down) and swirl that around until the goo is re-dissolved, then freeze and cross your fingers.

 

[musicguy24]

Okay cool, I was guessing lid off haha
I've heard of drying in the fridge?(No food in fridge)
You think drying out by a window would be better?
Is it too late to evaporate some naptha after you do freeze precipitation? And then try to re-freeze? I know that's not the ideal method, but if you're in the current circumstances of SWIM...
Thanks for answering my noob questions. You are awesome!!!

Well it really doesn't matter where it dries as long as it gets good air-flow. For this reason, by a window or under a fan is what works best for most. Just leave it in an open area and try not to let it collect dust or dirt from the air. (so don't leave it out on your back porch)

Yea that's fine if you want to evaporate down some before re-trying the freeze precipitation. That's called a "re-crystallization" and isn't necessary unless you need to rebuild gooey crystals or make a more pure product. In your case, I'm guessing you have a sticky goo on the bottom of your jar/spoon, so just heat up like a shotglass worth of naphtha(so you don't have to evaporate any down) and swirl that around until the goo is re-dissolved, then freeze and cross your fingers.

Alright gotcha!
Would it be okay to put it in a large bathroom to dry with a fan that sucks air into it lightly?
Okay awesome!! SWIM was planning on trying out re-crystallization.
Thanks for the explanations

 

[musicguy24]

Thank you Icon!
Thought I'd update on how SWIM's extraction went.
Bad news is that SWIM didn't get any crystals on the first 3 pulls from the lye/MHRB mix probably because of excessive jar moving around? But on those pulls SWIM is letting the naptha evaporate down and then trying to freeze precipitation again.
Good news is that SWIM still had one pull left to do from my lye/MHRB mix and after finishing everything and just leaving it alone in the freezer for 3 days it yielded probably around 150mg. Which I'm thinking is pretty good considering it was the last pull and SWIM is only dealing with 50g of MHRB.
This leaves me to wonder if SWIM didn't move around the naptha in the mix enough on the first 3 pulls and if SWIM should try doing anymore naptha pulls on the left over lye/root bark mix?
SWIM is planning to make Jungle Spice with the remaining mix, but maybe SWIM should do more pulls with naptha first?

And by the way SWIM smoked the ~150mg in 2 sessions, and it sounded VERY INTENSE!!
Everyone on this forum automatically deserves some serious respect for being able to handle this trip.