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official extraction help thread

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SWIM noticed that heat greatly help to separate layers. However it is not that easy to heat safely a big ammount of lye+naphta (very dangerous) :? SWIM thought about using an aquarium heater for that purpose.
 
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there were 4 layers (small layer of ms, small layer of what looked like fat, pinkish-brown layer and then the base layer). added 200mL water and 6 tsp of lye, but this is the fifth time to have done that...and remember, it was separating 36 hours ago.
 
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rainbowserpent - what tek are you using? mardybum - food grade plastic buckets work for large quantities though my friend prefers to work up his kilos in five batches of 200g each in gallon pickle jars and compare different techniques. There is a lot of evidence showing that too much lye and not enough water is what results in the thick goop that some have had trouble with. Note that I'm talking about in the basified solution, not an emulsion after the naptha is added. It seems like all that lye (in a recent account someone used my tek and due to a typo added four times too much lye) liquefies the bark and forms the sludge. If naptha is added before this is fixed, you'll get an emulsion from hell to boot. Adding more water is the only way I can think of to fix this - at least from what I've heard. The Antarctican has yet to experience this himself.
 
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[quote:4ee5ebf4bd="rainbowserpent"]the quicktek did a dry naphtha wash, then basified and added naphtha.[/quote:4ee5ebf4bd] Which quicktek? You're not narrowing it down much. The lazyman's is the one that calls for the dry wash if memory serves. I really wish you guys wouldn't make everything so goddamned hard with your dry washes and turpentine defats. Start simple and complicate from there to solve problems as they arise.
 
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[quote:70c7bce560="Noman"][quote:70c7bce560="rainbowserpent"]the quicktek did a dry naphtha wash, then basified and added naphtha.[/quote:70c7bce560] Which quicktek? You're not narrowing it down much. The lazyman's is the one that calls for the dry wash if memory serves. I really wish you guys wouldn't make everything so goddamned hard with your dry washes and turpentine defats. Start simple and complicate from there to solve problems as they arise.[/quote:70c7bce560] appreciate the comments, however utilized a pretty uncomplicated method. The bark was already powdered, so naphtha was added until it made a slurry, then was poured through a filter until mostly dry. The naphtha was evaporated (with obvious fat in it), and a mixture of 1L H20/8.5tsp (~40g) NAOH was added until the mixture was 1/4 bark, 3/4 mixture. The first pull went well, and the second was allowed to sit overnight. Over the course of the night, the layers went from separated to 4 layers (naphtha, fat, pink pubbles, black). At this time, the dmt-nexus was consulted, and the basic decision was to add more lye, which was done. Over time, several increments of 3tsp lye, 100mL h20 were added, but after no results and over 24 hours, more H20 was added, due to new comments on the situation from the nexus. At this time the mixture had to be separated in 3 different containers, as the H20 couldn't all be added to one, and part of another pull was evaporated off. If you can follow that...now there are 3 jars with pink emulsion that have since been dilluted with no results...the author is entirely sure there is more naphtha in them, but they won't separate. In light of the comment about keeping it simple, this time, due to prior experience, the method was kept VERY simple...no acid-base, no turpentine defat, no water wash.
 
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It has to be the dry defat that's causing this. Its the only thing out of the ordinary that you're doing. MHRB does not need a defat of any kind. Period. How much spice came out of the first extraction? For the rest of it, I'd add a lot of water - like bring your volume to double whatever it is now - and then run the whole mess through an old t-shirt or kitchen towel and squeeze the hell out of whatever solids get filtered out.
 
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that could be. Hrm...read a suggestion someone put up about making a single-best-type of extraction, and kind of think that needs to happen. I've used 3 different pdf files from this website (elfspice, vortex, normans), and apparently they all have misprints and misinformation. Not complaining at all, just thinking that for whoever starts up next, at the very least, they should know what works and what is more experimental. added about double the amount of water, and was able to get some goo out of the second pull (by adding TONS of water, a LITTLE BIT of naphtha was separated out and evaporated. This is a blackish goo compared to the yellowish goo w/ white and yellow crystals had on the first pull. Still, why would a dry naphtha defat not hurt the first pull, but hurt the second? I'm trying to figure out what went wrong, because this extraction is (pardon my french) fucked. There are several different colored layers...luckily decided to do a small 50g mimosa extraction so not too much was lost. want to try again, but have no idea what to do...believe you Norman, after all, was using part of your tek, but heard from several different people you can't overbasify and apparently that isn't true.
 
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[quote:db5de5dece="rainbowserpent"]I've heard from several different people you can't overbasify and apparently that isn't true.[/quote:db5de5dece] You didn't hear that from me because I had no idea if it was true or not until last week when I heard from someone who had most definitely overbasified. I think that what happens ((I'm guessing here) is that the bulk plant material gets dissolved into the solution and creates the nasty soups we've been hearing about from other straight to base extractors. Probably generates some nasty emulsions and dirty sticky hard to clean spice too. The problem seems most pronounced with pre powdered bark, probably because its ground finer than we can at home with a blender. From pictures I've seen, the pre ground stuff doesn't have that wooley fiber that's always left with a blender. Maybe pre ground bark is just a bad candidate for straight to base teks. At any rate, your problem wasn't over basification. At least not at first. Regarding that first pull - how much spice came out of it? How much naptha was used? How much naptha came back out? Was the base solution clear black or cloudy? Were the solids floating or sunk to the bottom? BTW - is there a typo or misinformation in the PDF of my tek? I know there was a typo in the first version up here but that was fixed. If you try it again, make sure you're using the "as edited by Zhah" version.
 
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the first pull utilized around ~150Ml of naphtha, and produced 3-4 'globs' of yellowish-brownish goo with white and yellow crystals. One of these globs sent me on my farthest journey ever! Do you think that the naphtha leftover from the dry defat could have caused a problem slowly as it went from slightly acidic/neutral to totally basic? The basic solution was clear black, but impossible to see through...no solids at the bottom.
 
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[quote:66ddf53673="rainbowserpent"]the first pull utilized around ~150Ml of naphtha, [/quote:66ddf53673] Do you think that 150ml came back out? I'm thinking that there was naptha from the defat left in the bark and that it slowly sucked your extraction naptha back in. This powdered bark sounds like weird shit. My friend has yet to work with it but I'm starting to suspect that reducing what would remain wooley fiber in a blender down to powder makes it way more subject to emulsions. Probably because those are structural fibers in the plant to begin with.
 
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I sure hope it isn't the powder root bark causing emulsions. The first extraction turned into a nasty emulsion after the first pull, but I thought it was caused by stirring the naptha into it. Second extraction yeilded tasty crystals using a simple A-B method. The third extraction is going to be Nomans using powdered bark once agains. Would you think it will be fine if the jar is just rolled around instead of stirring like the first time
 
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A person who sends me letters with no return address for reasons not understood let me know that their third extraction (all extractions have been very small scale) is looking to be the best yet! The most recent extraction was the marsofold tek. after all of the pulls, etc, the letter writer wrote that he/she/it did 3 pulls which resulted in approximately 30% more naphtha than the tek specified. the letter writer does own a baking pan, but it was in use for food, so the writer sealed up the mason jar and put in in the freezer. After less than 2 hours the mixture became cloudy and crystals formed, and the writer wrote that in the morning there were MANY white crystals in the mix. Apparently this thrilled the writer, as they were not having much luck, and were not sure what to think with the extra amount of naphtha. Anyway, the writer has a couple of questions.... *first, the writer has never freeze-precipitated before, and is a bit afraid of screwing up at this point...when it is time, the writer plans on doing the separation as fast as possible in a freezer, but once the naphtha is poured out, what should the writer do? should the writer seal back up the jar and take it out of the freezer? should the writer leave it upside down in a freezer for a while until the naphtha is gone? what about the filter paper that the naphtha will be poured on to? the writer is afraid of condensation on the filter and/or on the jar...also, the writer is afraid of the naphtha on the filter paper heating back up as it is drying and melting the crystals. The writer realizes there will be more crystals in the solution and plans on evaporating most of that off after this procedure and doing a second freeze precipitation....the other thing is that the solution seems to be staying cloudy (expected). Should the writer let the solution warm up to room temp and evap down or should the writer take the precipitates out and then evap? The solution is in a mason jar (~75mL), so the writer is afraid of moving the solution too much (jar->dish->jar?). ...could really use some help, can't find the information this person is looking for and will surely screw up this step without the knowledge of someone who actually knows what they are doing...!!!!
 
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Ok - don't worry too much. Just act fairly quickly and you won't lose anything. Perhaps the simplest method is to take the jar from the freezer, open and scrape it all around with spoon or something else suitable until all (or most) of the crystals are floating free. Then pour out through a filter paper into another receptacle. Let it drip a few seconds and then re-seal. The crystals in the filter will be fine - just let them dry thoroughly. Once the jar has returned to room temp, you can open it and let the remaining naptha evaporate - to see if there is anything else left of interest. Generally you'll get most of what you want in the filter.
 
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You will want to suspend a coffee filter across the mouth of a larger jar and pour your solvent through it a quickly as possible, then upend the solvent jar and let it sit and drain until it comes to room temp. Like the pic I posted on page 2 here: http://www.dmt-nexus.me/phpBB2/viewtopic.php?t=460&postdays=0&postorder=asc&start=15 Once your jar is at room temp, remove it and fan the inside to dry up any remaining solvent , spread the filter out to dry, and scrape out the jar with a rubber spatula.
 
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grazie!!! :D Upended into another jar, but the cooled mineral spirits didn't all make it into the other jar, probably 1/6 of it spilled out...heard the writer was using 2 filters, which might have caused the problem (mineral spirits laying on the filter.) Still, the writer appreciates the help with this so much! The writer would still be making blackish gunk with the QT tek if it wasn't for the smart minds drifting by. :) --edit--- the crystals dissolved back into the mineral spirits :( that's what the writer was afraid of...suppose time will tell...
 
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Is this writer using naptha or mineral spirits? They should have ended up with a jar of solvent on the bottom, an empty upside down jar on top with spice stuck to the sides, and a coffee filter with some spice in between. Where was the spice in contact with the solvent to allow it to redissolve? Try just pouring most of the solvent off the crystals (through a filter to catch strays) so that one ends up with a slush of solvent and spice and then evaporating the slush.
 
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the writer is using mineral spirits. He/she/it ended up with a jar of solvent ~10-14mL less than before, VERY wet filters, and a jar which had crystals that redissolved while the jar was upside down (when it hit room temp). The writer thinks using 2 filters might have hurt the process, as the mineral spirits were sitting on top of the filter (how some poured off). With any luck the crystals will come back in the jar and there will be some on the filter. will let you know whenever another letter is sent this way.
 
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