Weird : DMT crystals do not dissolve during second wash ?

[happydonkey]

Hello,
I did a successfull mhrb A/B extraction. And then decided to carbon wash to have a cleaner result.
After the first wash/freeze recrystallization,I was still not satisfied,so I did a second wash, dilute the crystals in warm Naphta,without any problem,I added the sodium carbonate mix (very little carb pH ~9.5) tap water,mix all.go back to work while decanting.
Just a normal, classic procedure.
But when I came back,I saw a lot of particules floating. Tried hot bath : nothing, so I filter the solution got the particules wish are clearly DMT, put them in new warm naphta
They remain the same ! Not dissolution ... What's that ? I'm really curious it's the first time I see the behaviour.
What could I do to get my spice back ? Any suggestion is welcome

 

[downwardsfromzero]

How are the particles so "clearly DMT"?
Do they dissolve in deionised water?
Are they soluble in ethanol?
At what temperature do they melt?
How do they react with vinegar?
What if they're in fact calcium carbonate? (You used tap water and added sodium carbonate...)

 

[happydonkey]

Shiny, yellow, crystal like and definitely smelling the good stuff when burned.
They dissolve in vinegar, I don't have any ethanol.

I didn't try either to dissolve them in ~ph7 water. But that's an interesting point, you mentioned several time ionized water.
Could the difference between tap water and distilled water make such a difference (chimicaly speaking)?
I thought it could impact (very slightly) the first acid extraction, but would not transform the future freebase?

Since they dissolve in vinegar, should do redo the all process (acid —> base > naphta pull? Do you think that would be a clever way to get back to normal?

 

[downwardsfromzero]

Well, that sounds like DMT. Some photo's of your process would really help.

Yes, you can pick the crystals up with vinegar, base that again and pull with naphtha. Try to use distilled or deionised water when making up your base solution because insoluble salts from your tap water may have caused a problem here.

When you said "dilute the crystals in warm Naphta" does this mean they completely dissolved in the naphtha prior to the sodium carbonate wash? If the crystals didn't dissolve then the puzzle continues. They may have become coated with an insoluble salt when you performed the sodium carbonate wash which would possibly make them difficult to dissolve in naphtha.

If you perhaps have some vodka it would be worth seeing if a small sample crystal dissolves in that, just to be sure.

And DMT freebase should melt between 46 and 60°C depending on the polymorph. It can behave a bit oddly at times!

 

[happydonkey]

Thanks for that detailed answer

Yes, before that gap, the dmt dissolved entirely in naphtha, then I added the carbwater, then it sort of recrystalise in the carbwater-naphtha soup :?:

I never heard about the vodka trick, what would it demonstrate?

Yes, good idea, I'll post a pict of that phenomenon tomorrow, could be interesting for someone else. (just too lazy right now , it's almost 3am after a long working day

 

[downwardsfromzero]

From what you say, it seems pretty clear that you do have DMT. Maybe your initial crystals were fairly large and well formed. That would slow down the rate of dissolution quite considerably.

When it refused to dissolve in the naphtha, what temperature were you using? Was it cold? Did you try warming it? Did you try crushing the crystals? Was the carbwater warm or cold? Adding cold water to a naphtha solution of DMT could cause the DMT to precipitate.

I never heard about the vodka trick, what would it demonstrate?

Really, this is talk for another thread but the mysterious behaviour of your crystals spurred me to try roping you in on the experimental side

DMT freebase should dissolve in aqueous ethanol - which is pretty much what vodka is. This is current research so I'm just fishing for new data

I've only tested DMT freebase solubility in ethanol between 90% and 50% ABV - it was very soluble within this range - while also finding that 20% ABV was insufficient to noticeably dissolve it. Vodka is typically 37 - 40% ABV, just past the mid-point between insoluble and very soluble.

What the 'vodka test' may be able to indicate is if your crystals dissolve in vodka and then precipitate again, either with cooling or after careful addition of a few drops of distilled water, then you have something with a solubility characteristic similar to DMT. [It may precipitate as a yellow oil as DMT seems to have a very high affinity for ethanol. Slow evaporation of the ethanol from this oil at -18°C provided off-white crystals.]

Eventually I'll do the experiment myself although progress tends to be slow here at Zero Towers.

 

[happydonkey]

me to try roping you in on the experimental side Very happy

But indeed you succeed :lol: :thumb_up: because right after asking I searched for that info, but your explanation is completing the one I found, since there was a part missing :

Slow evaporation of the ethanol from this oil at -18°C provided off-white crystals

which could be a nice tricks to try ;-) Probably next "normal" wash, not cumulate the difficulties (or maybe 50/50 !)

But I think, you point out the prob :

Was the carbwater warm or cold? Adding cold water to a naphtha solution of DMT could cause the DMT to precipitate

Exactely what I did, on the ~35° DMT-Napthta I add the carbwater just made from tap, and this one should be at around 10°C ... almost 25°C delta.

Since you are interest on vodka feed-back, (almost .. 50° Rhum room temp), it dissolved in less than 5min, I dont know exactely, I just left, came back and dissolved (ok it was a very small sample ...)

Some compiled pictures

 

[downwardsfromzero]

Yeah, it seems like the cold solution crashed some crystals out from the naphtha and maybe they got coated/co-crystallised with calcium/magnesium carbonate if you've hard water in your area. Nice to have had a little mystery to attempt solving

Thanks for testing out with alcohol - I guess 50° equates to 25% ABV? It looks like you used a large excess of the rum, which makes me wonder how well the DMT would dissolve in a far smaller volume. This is an experiment for me to do as it would be unfair to ask you to keep dissolving your precious product - unless you've got bitten by the science bug for this too! :twisted:

 

[happydonkey]

Sorry,I didn't try the small amount of Ron,but maybe it's not too late for the next wash

I proceeded as follow :

From the funnel,I separated the layers,collected the solid part,freezed the naphta and got few nice crystals, but that's the normal part.

But I filtered my other naphtha jar with the undissolved crystals.
I added those,with the solid one from step one,and put them all in a acid ascorbic solution.
They dissolved, .... coool ;-)
Then I added slowly a diluted lye solution (funny white clouds in the watter) until ph11
Everything was still diluted ( I think)
Then added some clean naphtha, put it on a magnetic stirrer, for maybe 15min
Let it separate
I planned to do a classic freeze recrystallization,but what the fff!!! When I came back, I discovered 3 layers : napthta,a very red??! Water and a thin layer of crystals,wish I'm pretty sure are DMT ! (CF attach)

I definitely won't say that I'm a DMT extractor expert 8) but I did a couple of extractions/wash testing different Teks,but I found the current behaviour pretty fascinating :shock: