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Questions about residual naphtha after freeze precip (Extract problem) Options
 
Synergy
#1 Posted : 7/18/2012 1:47:36 AM
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Ok, so SWIM has done a few extractions now and is learning new things every time. He thought he might need you guys the first time but he ended up just evaporating and it was kindergarten simple but obviously created a more yellow product. There is one thing that kind of has him hung up though. He's read a lot of TEKs about freeze precipitation and has only attempted it once. The reason he's only tried it once is because when he did it he ran into a small problem.

He used a small mason jar and was using naphtha following a couple simple STB pulls from MHRB. He let it sit for nearly three days and had plenty of gorgeous white crystals with a tinge of yellow in them stuck to the bottom and sides when he pulled it out. He already had a coffee filter set up over a secondary mason jar. He quickly unscrewed the airtight lid and started pouring the naphtha into the second jar. The coffee filter collected a decent amount of floaters and the rest stuck to the jar.

He then placed the lid back on the first mason jar and tipped it upside down in the freezer to attempt to let any residual naphtha drip and settle on the lid. When he went back to check out the jar after 24 hours, disappointingly the crystals had turned into clumps of off white wet powder/goo mix which still appeared to be pretty wet. He left it in there for another 12 hours and it had the same exact look when he checked it again. He unscrewed the lid and strained a good bit of naphtha that had dripped down and formed more of the same off white powder/goo on the lid.

He did this a few times (more naphtha and/or moisture continued to settle on the lid). He tried to take out the jar with the lid off to let the powdery goo dry so he could scrape it cleanly. As he watched the jar he could see the powdery goo dissolving and more liquid/naphtha forming seemingly out of nowhere (where the looked to be none before). He put it directly back into the freezer after witnessing this.

He ended up just scraping the sides of the jar directly after taking it out of the freezer while the off white powdery goo was still moist and had to let it all sit and evaporate on a plate. A good half of it or more turned to liquid shortly after being scraped and put on the plate. This was very frustrating. When it was finished evaporating he did have a cleaner product than he got from evaporation without freeze precipitating but it took MUCH longer and he's wondering where he went wrong. He didn't evaporate any before placing it in the freezer the first time because it was a pretty small amount of naphtha to start with, the pulls came from 1lb of MHRB, and he thought it it was already saturated enough. He's also wondering how he can avoid those gorgeous crystals transforming into powdery goo (which when dried, turned to a very flakey, grainy, off white powder).

SWIM realizes he's probably making this a lot more complicated than it needs to be and probably just did one thing wrong or could have done one thing better. Also, he wants to note that the finished product was very very active and definitely "good" but not what he expected from reading other TEKs and seeing other pictorials. Any help will be greatly appreciated.

Edit: Also, I just read about someone on another forum having an eerily similar problem. They said they thought that the xtals were holding residual naphtha behind them and when it was warming to room temp it was transforming the goods. Now after they witness the xtals stop growing, they take out the mason jar and violently shake the jar for a few seconds to remove the xtal growth from the bottom and sides and use a metal tool to remove any still stuck so that they are now floating in solvent and just filter it immediately. Would this help keep those nice xtals from transforming into anything else or would they just melt into the coffee filter or still transform to powdery goo due to not being completely dry of the naphtha and cooling to room temp? SWIM is trying to figure out how to manage this problem because he still has a good bit of base MHRB solution sitting that he believes has at least a few pulls left in it.
 

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SeekerOfTruths
#2 Posted : 7/18/2012 8:30:40 AM

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This is just my best guess as to whats going on.

First off I find you need to have your freezer VERY VERY cold, like the coldest setting right next to the air vent.

Extracting from 1lb of MHRB in a single container seems like a lot to me, here is a picture of an 8 cup pyrex dish from just 150g of MHRB

Now the Pyrex dish will have a lot more surface area at least in terms of gravity with the crystal formations, therefor the crystals should be smaller, and smaller crystals should have less of a chance of trapping solvent inside of the crystalline structure. But A mason jar on the other hand has far less surface area for the DMT to latch onto and I'm guessing your getting larger crystals. Plus you're pulling from nearly twice as much MHRB as I was, and you can see my dish was pretty much coated.

When putting the dish in the freezer I cover the pyrex dish with saran wrap or foil (I think foil actually works better i'm finding). Then put the lid of the pyrex dish on. After this I put the container into a ziplock (carefuly as to not spill the anything, the lid may not be 100% air-tight).

I've had no issues with anything turning into liquid or anything, but I also wait until its completely dry. As I mentioned on the other thread, after pouring the solvent off I let it 'warm up' in the refrigerator for about an hour, then I transfer it onto a sheet of tin foil, upside down with a small glass or shot glass propping one side of Pyrex dish up so that some airflow can get to it. I cover this with a bath towel to let the temperature raise slowly as to avoid condensation, and usually within 12 hours the pyrex dish will look exactly as the picture above but it will be dry. Then you take a razor blade and scrape it out.
 
endlessness
#3 Posted : 7/18/2012 8:53:07 AM

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You can just redissolve the goo in warm naphtha or ethanol or IPA and let it evap in a wide dish, it will solidify with time (just scrape/re-scrape, move it around a bit if it stays as a goo)
 
Synergy
#4 Posted : 7/18/2012 9:10:16 AM
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endlessness wrote:
You can just redissolve the goo in warm naphtha or ethanol or IPA and let it evap in a wide dish, it will solidify with time (just scrape/re-scrape, move it around a bit if it stays as a goo)


I've been talking with seeker about it a bit in chat and he's given me a little advice I'm gonna try. I mean I'm not left with a goo in the end. It's an off white flakey powdery substance in the end. I just hated watching those nice white big xtals turn to that and not knowing why it wasn't as easy for me to decant and dry ALL of the naphtha and be left with those xtals without it transforming them into what it did. It was like in the mason jar it was almost impossible to get out all the naphtha for me, which led to redissolving spice when heated to room temp to try to dry out the gooey powder, which then led to me having to put it back in the freezer and later just end up scraping it without it being completely dry. Then having to evap the naphtha/dmt mix (which was just enough to dissolve about half of what I scraped onto a plate prior to evaporating and drying).

It was a fairly clean end product, but definitely not the xtals I saw at one point during the freeze precip.
 
heavyhanded
#5 Posted : 7/19/2012 4:03:31 AM
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I'm having very similar issues due to the use of pint jars. Never again.

My question is how much naphtha to use to redissolve the crystals in the jars I currently have upside down, but can't harvest from. I don't want to use too much and wind up with unsaturated naphtha.

I asked this in the general help thread but figured it wouldn't hurt to add it on here. Thanks again for any and all input!
 
endlessness
#6 Posted : 7/19/2012 9:22:13 AM

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Warm up naphtha (Safely as FAQ says) and add it slowly so you'll know when just enough to dissolve it all has been added. Then you can add a bit more after you've poured off, to pick up last traces.

Be well!
 
 
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