Yesterday, I ran into something that I haven't seen happen yet. 7 jars of NaOH solution were made by using 1500mL of distilled water and 100g of NaOH. pH of 6/7 jars read 12.2-12.3. The jar in question had a pH of 11.9. I figured that it was close enough to a pH of 12 that it would be fine to continue. 100g of MHRB was added to each jar and all jars were shaken well and left to rest over night. 10 hours later, 100mL of VM&P Naphtha was added to each jar and jars were turned end over end, left to separate and repeated a total of 3 times. After the third separation I began pulling the solvent from the jars. There was a slight emulsion in the jar with the lowest pH so Without checking pH, a small amount of NaOH solution was added to the jar. The jar was turned end over end a few times and left to separate. The emulsion had started to break apart and yellow crystals began appearing on top of the emulsion.   The first solvent pull was retrieved from this jar and placed into a separation funnel with the first second and third pulls from the other 6 jars. Today, the emulsion is gone and and there appears to be a lot more of these yellow crystals suspended between the solvent and basified extract. The pictures don't show it but it looks like a layer of gold flake.   A small amount of baseified extract was retrieved and pH measured reading 12.1  Some of these salts(?) carried over from the first pull and into the extraction.   Yesterday, when I asked a good friend I was told to carry on with the procedure and while I trust his advice and the advice that was given to them, I'm still left with a few questions. 1. What is this? It looks like a very shiny salt. 2. Do I need to get this out of the extraction? I'm confident that I can remove this either during or before washing the solvent if I need to. 3. Why did this happen? Thanks for taking the time to read this and thank you for any insight you may have.
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Im considering the possibility it is DMT which crashed out of your saturated solvent as it evapped/cooled during the extraction/mixing, but since freebase DNT isnt water soluble it just stays there undissolved on the bottom of the non-polar.
If that is the case, it will probably dissolve once you start doing more pulls with fresh solvent.
You can filter your non-polar from your first pull which has the floating crystals, and keep it separate just in case.. Then you can proceed with the extraction. If it is DMT it will dissolve in fresh solvent. If it doesnt, Id keep it separate and you could run some more tests, like for example do a reagent test on it or whatever.
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I've had the same thing happen a few times with crystals forming on top of the based material layer like that. I think what is happening is as the solvent cools, the DMT crashes out and sits on top of the base layer. Adding heat has worked well to get it back into the solvent for me.
Are those crystals stuck on the sides of your sep funnel? They are DMT too I believe. That happens to me when I let solvent from pulls sit in a glass container long enough, or sometimes quickly in my glass pipettes when they are cooler than the solvent I'm pulling through them. Heat will help here too getting crystals to melt back into the solvent.
One of the DMT crystal forms is salt or tiny prism like in appearance.
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endlessness wrote:Im considering the possibility it is DMT which crashed out of your saturated solvent as it evapped/cooled during the extraction/mixing, but since freebase DNT isnt water soluble it just stays there undissolved on the bottom of the non-polar.
If that is the case, it will probably dissolve once you start doing more pulls with fresh solvent.
You can filter your non-polar from your first pull which has the floating crystals, and keep it separate just in case.. Then you can proceed with the extraction. If it is DMT it will dissolve in fresh solvent. If it doesnt, Id keep it separate and you could run some more tests, like for example do a reagent test on it or whatever.
Thanks for the advice. I'll extract the first pull and see what happens after adding new solvent. If the crystals don't dissolve, I'll put it on hold and buy some reagent tests. I've got some Ehrlich but I think that I need Hoffman for this.
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Pictured here are the crystals in DMT saturated VM&P Naphtha. They are very enjoyable to look at and remind me of diamonds.  The solvent was washed once with Sodium Carbonate and then twice with distilled water. Some of these crystals sank to the bottom of the separatory funnel. I didnt take a picture but not all of then sink. Some of them float in water too.  The wash water was filtered with a Bunchner filter and the crystals collected.   The crystals were then rinsed a few times with distilled water.  The crystals were then placed in a ceramic dish along side known DMT and tested with Ehrlich reagent. DMT on the left, mysterious xtal on the right.  The DMT dissolved immediately but the crystals took maybe 30 seconds to fully dissolve. Both turned purple immediately. This stuff doesn't dissolve in new room temperature solvent, and it doesn't dissolve in chilled distilled water. If this is DMT, how did this happen and why won't it absorb into new clean solvent?
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Beautiful pics! Definitely DMT if you ask me. That crystal type reminds me of diamonds too and I agree are very enjoyable to look at and not as common as the other types.
They will dissolve/melt back into solvent eventually if it's warm enough. If you put those into a container with solvent in a heat bath, that would do the trick. Someone else who knows more about chemistry and crystallization than I do could probably explain in more detail exactly why that happens.
I personally like the diamonds and would keep them that way if it was mine. IME those type of crystals are dense and weigh more than it looks like they will once dry.
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That was quick! Cool that you seemed to have answered your question! Thanks Doc & endz. Cool thread. 
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The "diamonds" are pretty dense but they're difficult to extract. Part of the emulsion remains making it difficult to pipette and because this is STB, the plant matter males it impossible to use a sep funnel.
I may try to reproduce this using a smaller amount of raw bark powder but it's bothering me that I still don't understand why exactly this happened. This was the only 1/7 jars made at the same time from the same material and that resulted in this phenomena.
What we know: 100g NaOH was added to 1500mL distilled water in a glass container. pH of solution was 11.9 and solution left to cool to room temperature. 100g Minosa Hostillis root bark powder was added to solution and shaken vigorously. Container was left to sit for 8-10 hours. 100mL of VM&P NPS was added to the basified extract and the container lightly turned end over end and left to sit for 1 hour. A minor emulsion was observed between the NPS and base. An unmeasured (but small) amount of NaOH solution of pH 12+ was added to the basified extract. Diamonds began to form immediately but the count increased over a 16 hour period.
So.... what's going on here?
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It might simply be a polymorph of DMT that has lower solubility in the non-polar solvent, or it might be NMT, though its generally only in small or trace quantities in MHRB. My guess is its a DMT polymorph. Either way the ehrlich reaction shows pretty clear its an indole based alkaloid. Id use warm solvent to redissolve it. You should continue the extraction as normal. You can keep those crystals separately if you want, to do more tests or whatever.. but you should be fine mixing and consuming/smoking with the rest if you want too.... TLC would answer more definitely what it is.
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endlessness wrote:TLC would answer more definitely what it is. This is bad ass. Thank you.
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