OK here are some thoughts on your earlier question.

IME and IMO, No. You are going to lose quite a bit of your other alkaloids when attempting to purify it further after you have done you initial freebase conversion.

After doing you initial freebase conversion you have jungle FB. Anything you do after that that involves Naphtha or Heptane is going to clean the jungle out of it. I honestly dont know about Xylene.

Convert from fumerate to FB and leave it as is. IMO it is as good as it gets at that point, well, at least as far as the effects are concerned. Some say white tastes better. If your making changa out of it it doesnt need to be cleaned up at all. Done.

endlessness answered it up in #135

Thanks, I ususally aim for white crystals butI guess I'll have enough of that from the white fumarate once its converted so I'll give the 'full spectrum' freebase a try. If I don't like it I guess I can always redissolve it in water, pull with heptane to get white & then pull the remnant with Xylene to get 'pure' red jungle spice (though I'm not that fond of it).



He was answering xibalbaNOW's question.

to clean fumarates you can recrystallize with IPA or Acetone.. Just redissolve it in warm IPA/Acetone and freeze it. It will at least get rid of limonene remains (which should stay in the solvent after crystals re-precipitated). Make sure the IPA or acetone are dry, otherwise your fumarates might not crash

I'm going to do that with the dirtiest of the fumarate tonight & just freebase the cleaner yellowy fumarate.

I've redissolved in warm IPA, but not all of the fumarate has dissolved. I'm not sure of the reason. Presumably some isn't dmt fumarate, but I don't know what it could be other than fumaric acid though I'd expect it to dissolve too.

Any idea?

maybe its not enough IPA or its not warm enough? dont throw anything away before you have your final yield, as it might be your alkaloids there. And fumaric acid would also dissolve in the IPA

you could try freezing for a couple of days the pull you made already, and then add more hot IPA to what was left behind and freeze that separately.

I heated the IPA & managed to redissolve it then crash out the fumarate alkaloids. Its looking a good bit cleaner now.

On a slightly seperate issue I've got a very low yield in conversion of the pure white & slightly yellower fumarates to freebase. I had 8.4g of white fumarate (albeit not fully dried when I weighed it) & this converted to 1.25g of freebase. I also obtained 400mg of yellower freebase from my seperate pile.

Even taking into account the fact that the 8.4g wasn't dry when weighed this is less than I was expecting. I've saved the Sodium Carbonate water used in the conversions & this is still very white. Is this normal or is this an indicator of significant DMT still in it?

I put a few pippettes of new sodium carbonate water into it and it got a little bit whiter in spots - not very noticably though. I've put it in the fridge again to precipitate out whatever might still be in there but if the white colour indicates plenty of DMT still in solution (I hope so) why didn't this crash out after almost 2 weeks in the fridge? And how can I ensure it does so?

Thanks

how long did you wait for the conversion? (edit: sorry you said 2 weeks... that should have been more than enough) How much bark was it to start with, for those 1.25g+400mg ?

Try putting the water in the freezer, let it freeze and thaw and see if more crashes out. Lastly you can also try doing a small pull with a solvent in that water and salting again to see if something comes off, but I would guess with long fridge precip, then freeze and thaw, there will be very little, if anything, that isnt precipitated

It was 450g bark. A previous extraction with the same bark gave a yield of just under 2% (though by a different tek).
I've got it in the fridge now, I'll try freezing it for a while then a solvent pull.

Edit: should make clear the 1.85g isn't all from the 450g- I've got some fumarate from the same batch drying now.

I just found this tek in the FAQ and I cruised through several pages. Has anyone tried this with ACRB? I am hoping to find a good non-toxic that will work with this material.

Hey wait, HDPE is not compatible with limonene, from the table I looked at... PETE is tho.

^^^

I bought a gallon of limonene from Greenterpene around 7 years ago that came in a HDPE jug. Just went and checked, it has split along the seam, on the side of the container. The limo at the bottom is thick and dark but the plastic it's in direct contact with appears intact on casual inspection.

I want to do a batch with BLAB tek, and I have question about the amount of sodium hydroxide (NaOH) that it calls for. A year ago I did some experimenting with pH meter and found that 10.5-11 grams of NaOH brought 250mL of water to pH 12.5 or so. After adding any more NaOH than 11 grams, the pH started to go back down markedly. I did some research at the time and it all made sense (calculation with moles and ions).

Extrapolate my ratio to 3700mL and it should take 163 grams of NaOH to basify, so how is it that BLAB tek calls for 250 grams NaOH, even if the 3700mL starts off slightly acidic? I guess I could take the approach of don't worry about it and follow the proven recipe, but, you know, I'm losing sleep not understanding and asking here.

pH should simply go up with NaOH concentration. Maybe you where at the max range of the pH meter?

Remember too that a lot of pH probes just don't like strongly alkaline conditions. Refer to the instruction manual if possible. (This is basically the same as what Loveall said.)

Oook I guess I've been out of chemistry class for too long I did use an Apera LabSen 841 probe, which is specifically designed for pH 10-14, and calibrated per instructions, but maybe somewhere else in instructions it says to not use it with NaOH? Not sure, but at the same time the pH reading started to go back down, my adding of NaOH stopped showing any exothermic reaction.

Need to find an Alexander Shulgin inspired chemistry / organic chemistry course I could sign up for

Hm, sounds like your probe should be able to handle the conditions then. You were doing this with just water and NaOH were you? No bark added?

Is it in any way likely that your water might have contained a significant amount of dissolved CO2? It just sounds like there was something dissolved in your water which was exerting a buffering effect. What kind of water was it? Dissolved bicarbonate or phosphate might have this effect.

At step 5A, I have white crystals stuck to jar and poured off the D-limonene (as much as would pour off anyway). I opted to add water and transfer to crystallization dish, but I noticed separation layer. I'm guessing that a certain amount D-limonene will dissolve in water and that's what's on the top, and then on the bottom is absent of D-limonene.

Forgive me if I overlooked this and it has been covered before, but if I separate the layers and evaporate each, will DMT fumarate be with both the D-limonene layer and the water-only layer? Is there a way to separate the D-limonene and water that dissolved together without fractional distillation (if D-limonene had lower boiling point than water then I'd be set, but since water has lowest boiling point, I'm left with D-limonene which I'm trying to get rid of).

I understand there's all sorts of clean-up teks with basifying or washing etc, but I'm just hoping someone can satisfy my curiosity with questions above. If DMT-fumarate will exist in both the water and the D-limonene layers, I imagine evaporating the dish with no D-limonene will yield relatively clean crystals...

FWIW, after separating and evaporating, I got results in pictures. The gooey D-limonene fraction will get cleaned up over next couple days via NaCO3->evap->3 acetone pulls->add FASA->wait few hours->decant and dry and scrape... but it's nice that I have 80+% already clean and ready to go with less time/effort.