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What is SWIM doing wrong?

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I havent tried the freeze extraction in many years but unless your naptha is at the brink of being supersaturated then that naptha will still have some spice left. Freeze extraction doesnt recover 100% even cold naptha will still dissolve some spice albeit considerably less than warm naptha. If you have way more naptha than spice then you will definately have to evap off some. Remember to always keep your solutions until you are satisfied with your yield you can almost always go back. The goal right now should be to figure out where the spice is. Is it in the naptha or is it in the solution still. In theory it should be in the naptha but something could have gone wrong.

I would reccomend completely evapping off your naptha to see if anything results. If you have issue with evapping off naptha safely without making people nearby curious try taking a small percentage and evap that off. If it results in a decent amount of crystals compared the the percentage you vapped then you know where your spice is. Second make sure that your container is sealed when freezing you dont want water getting into your solution from condensation this can be a issue as well. Then there's always the possibility that your mimosa just had a bad percentage. it happens.
 
what naptha are you using? There should be no residue from naptha unless some of the chemical from the extraction is getting into the naptha or the naptha has some chemicals in it. Many versions of naptha has lubricants and other chemicals in it. if it's a part of the solvent then a wash or two should get rid of it. If it's lubricants in the naptha your screwed. You'll have to change the naptha you use but you wont be able to get that stuff out of this batch. It could also be binding the crystals in the solution as well. The best thing to do is take some pure naptha you have not used for anything evap it off and see if there is any kind of residue. If you see anything then it has other chemicals in it. Another thing that I would consider which I have no experience with but 'might' be a issue is if you are using plastic naptha might dissolve chemicals in that plastic as it sits. This is the reason why I only ever used glass for every single step.

I have 0 experience with DCM Remember it's been 5 years since I took on this. I havent done anything chemistry wise since then. DCM was discovered after my experiemnts.
 
No it's what I used back in the day. I think your good on it unless the formula changed over the 5 years. There is some residue from what I vaguely remember but not much. Once you get your evap off do a solvent wash like in my tek and it might get rid of that residue if it's basified solution. I made the wash because regardless of how well you think the seperation was done there will always be a microscopic bubble formation inside the naptha. If you look at my tek you will see in the bottom of the small flask all the crud I pulled out of what seemed like pure crystals.

I evapped my extraction. I only did freeze evapping on a experiemnt or two. It was just being developed right when I was doing my tek. The freeze process was discovered by a fellow deep thought member and what is in my tek is from his information. I didnt do much on freeze extraction myself. Plus it's been 5 years my memory on it isnt rock solid. Hopefully somone who has done work more recently might be of better use for you.
 
That's the right naptha. Although you did an A/B extraction, and you should need a ph of only 12.4, try bumping it up to the STB ph of 13.6. This may or may not help, but I don't think it could hurt.

Also, what temperature does your freezer get down to?
 
Some people seem to find STB to yeild better. I speculate this is because of the higher ph. But I would like to know from someone, is it a plausible idea that DMT can vaporize during the acid boil if it is to hot?

And I believe the ideal freezer temp is 0-5F. If your naptha evap and refreeze is unsuccesful, try raising the ph to 13.6 and then pull with bestine, which can be found at art stores as a rubber cement remover. Bestine evaps really fast and clean, and might make your freezer not necessary if it can't get cold enough.
 
s8championjgh said:
I think swim is going to try a stb extraction next time

what volume of naptha are you putting in the freezer to precip from?

you say 150ml 3-4 times.. into a flat bowl. are you putting ~600ml naptha in a bowl into the freezer? is it sealed somehow?
 
is the bowl seethrough? yeah you need to evap the naptha down until it is cloudy.

if you want a better purity.. I reccomend evapping the naptha completely, then adding just enough hot heptane to dissolve all the material. let it cool to being cloudy and then pop in the fridge, then freezer.

scraping crystals out of a bowl or anything curved will make you wanna cry. got anything flat?
 
s8championjgh said:
1) Boils 200 grams of mimosa powder in ph3 water in a stainless steal bowl. Does this 3 times, each time about 2 hours each. Final solution fits in a gallon jug perfectly.
Boils?

Dosn't Mimosa have a evap point of 50 degrees c ?
:shock:
 
SWIM believes that boiling probably vaporized the spice. Also if it gets too hot it will stay as an oil and you may throw it out thinking it was trash. SWIM used to do A/B and the resultant spice was very white but the yields were much lower than just an STB. SWIM's favorite TEK is to powder the spice and put it in a crock pot at a ratio of 1gr MHRB to 1gr Lye to 1.5ml water. Mix the lye and water before pouring it into the MHRB in the crock pot and then turn on the crock pot at medium heat. After about two hours add 100ml Naptha and stir it well a couple to a few times during the next hour or two.

Warm up a jar like a mayonnaise jar that is wide at the bottom and gets smaller at the top so that the thermal shock isn't too great and then using a wide mouth funnel pour the liquid from the crock pot into it until it is up into the narrow area at the top. You can let it cool some and put the lid on and mix it well. You'll have to take the lid off and wash it out since it gets dark brown mimosa junk on it. Put the lid on and let the naptha separate for maybe an hour. The smaller neck of the jar will focus the naptha and make it easier to lift off. Take a turkey baster and carefully lift off the naptha from the top. The nice thing about the baster is that it has a fairly wide mouth and if you suck up some of the red liquid all you have to do is hold the baster upright with the tip just under the surface of the naptha and the brown liquid will drop right out of it. Lift the naptha off and put into a baby food jar. put the lid on it and put it into the freezer.

Within a few hours there should be nice crystals. SWIM just pours off the naptha and puts it back into the brown liquid and then back into the crock pot for a few more hours for another pull. The yields are amazing and it's very easy and quick to do!
 
Looks like about 1%, could be more, may just be good MHRB though. I see that there was a typo in the ratios also. It's 15ml water per gram of each MHRB & lye not 1.5.
 
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