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.
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.
