Recrystalization NPS Low or high boilingpoint

[Jules_supertramp]

Hey there,
i can't really find the answer to my question. SWIM wants to purify his product with recrystallization and got two solvents at hand, one with a Bp as low as 40-60°C and the other one 60-95°C. Is a high Bp better as more DMT can be hold by the NPS at higher temeratures?

Another question is, how much charcoal best to use? Is it even worth doing that or does one loose product this way.

You might let me profit from your knowledge and experience. I would be super thankful.

Peace,

 

[Brennendes Wasser]

Regarding my obervations the lower boiling stuff that you have (C6 - C5 Alkanes = Hexane + Pentane) dissolves much less DMT, but also less of the impurities. Still the other one is just the perfect all-to-go Naphtha (C6 - C7 Alkanes = Hexane + Heptane).

So I would also stick for re-x with these higher boiling Naphtha. If you dont get the results that you want you may go to the one one with Pentane ...

Regarding charcoal I think you mean to remove more of unwanted stuff? I never heard that people do this with DMT :? so no idea how effective that is - these Carbon Surfaces are highly adhesive to a lot of high-molecular things, which often cause coloration in otherwise white compounds. By using charcoal / activated carbon these high molecular things can be adsorbed and thus create white products.
Still no idea if this would also bind to DMT, but as nobody is using this as I guess, you should probably better try it on your own.

Maybe dissolve 100 mg of DMT in Naphtha, place Charcoal inside and either heat a little up or stirr manually and then remove the Charcoal and check upon evaporation if still 100 mg are retained. That could maybe be useful to know, as this may indeed get rid of that yellow coloration of some spice ... but if you dont wanna do stuff, then I'd just stick to re-x with simply the high-boiling naphtha - which is still regarded as low boiling considering there is Naphtha up to C11 - C13, which boils well above 200 °C. But that stuff is really not good to use with DMT.

 

[Bisy]

OMG! I just left a 15 minute reply and pushed the back button and lost it all. So this one is gonna be scaled down.
I'm just a greenie taking a shot at your question so regard it as such.
Its not bp that matters, its solubility at cold vs hot. U want low at cold high at hot. Im confident that the issue has been thoroughly explored by the best of the best and so safe to go with naphtha or heptane, as that is the current favs. Heat to near boiling in heat bath, vessel w spice, other w nps. Add sol slowly while swirling until spice no longer has any characteristics of solid or powder, but has a glob of darker goo at bottom. If you keep adding sol. It will dissolve but you dont want it to. You then pour off clear or slightly yellow so. Into new vessel. This can be done more than once if you want. When satisfied with color and purity, remove from bath and gently blow on it. It should cloud a lot and fast. If not, you need to reduce it some. After you achieve this, cover it and cool slowly. Room temp for an hour, if its freezing outside, move it to the garage for another half hour then refrigerator, and finally freezer for the rest of the day or night.

 

[Brennendes Wasser]

OMG! I just left a 15 minute reply and pushed the back button and lost it all.

Man thats bad :thumb_dow It also happens to me often when I'm jumping around in a comment with STRG + Arrow key and then I accidentally hit ALT + Arrow key. But then if I press ALT + other Arrow key (or just on FORTH on my browser) then I am back at my comment - possibly loaded from the Browser Cache or stuff. Maybe this will safe your life the next time or did you already try? :/

Also regarding the solubility issue:
Yeah that s really correct! But just regarding high-boiling Naphtha with more than 200 °C boiling point for example, you also could re-x at a given range, but this will not produce real crystals, if I have this correct in mind. I got more like a sludge or what and this was just linked to the longer Alkane molecules ... so at least in this case, even if solubility was super high when heating and very low in freezer, then these C11-C13 ones are still pretty bad for re-x.

Also if you already have that brown blob forming on the bottom, then indeed dont add anymore solvent. But still this blob will contain DMT, so instead of adding more solvent or directly decant it, stirr this brown sludge so you will whirl it in your solvent and get even more DMT out. This oily thing will act as a 2nd liquid phase and so you basically have a phase-separation problem with the DMT being soluble in both phases. Therefore the normal required amount of Naphtha wont be sufficient to get that stuff out. If you mix that brown thing like hardcore you may only need 1 or 2 pulls to get all your goodies away from the brown stuff, which will upon depletion most likely form a brown to even black residue, which will be even solid. Quite weird, that 2 solid things will form an oil upon combining :d

 

[downwardsfromzero]

(STRG is the German keyboard equivalent for CTRL, for those of you who were wondering )
I also find the browser cache (or whatever) keeps my reply window input when navigating back and forth with the ALT+← and ALT+→ keys. Maybe this is not the case for the mobile version?

High(er) BP naphtha can be a very good extraction solvent. Hydrotreated medium naphtha (sold as BBQ lighting fluid but this was 15 years ago) pulled very nicely when warm and gave excellent freeze precipitation results. It would be desirable to follow up an extraction that used high BP stuff whit a re=x or two from light naphtha.

Current thinking is that the brown blob is largely polymerised DMT; at a certain temperature it begins to dissolve. This was very baffling when I first encountered it.

 

[Jules_supertramp]

Regarding my obervations the lower boiling stuff that you have (C6 - C5 Alkanes = Hexane + Pentane) dissolves much less DMT, but also less of the impurities. Still the other one is just the perfect all-to-go Naphtha (C6 - C7 Alkanes = Hexane + Heptane).

So I would also stick for re-x with these higher boiling Naphtha. If you dont get the results that you want you may go to the one one with Pentane ...

Regarding charcoal I think you mean to remove more of unwanted stuff? I never heard that people do this with DMT :? so no idea how effective that is - these Carbon Surfaces are highly adhesive to a lot of high-molecular things, which often cause coloration in otherwise white compounds. By using charcoal / activated carbon these high molecular things can be adsorbed and thus create white products.
Still no idea if this would also bind to DMT, but as nobody is using this as I guess, you should probably better try it on your own.

Maybe dissolve 100 mg of DMT in Naphtha, place Charcoal inside and either heat a little up or stirr manually and then remove the Charcoal and check upon evaporation if still 100 mg are retained. That could maybe be useful to know, as this may indeed get rid of that yellow coloration of some spice ... but if you dont wanna do stuff, then I'd just stick to re-x with simply the high-boiling naphtha - which is still regarded as low boiling considering there is Naphtha up to C11 - C13, which boils well above 200 °C. But that stuff is really not good to use with DMT.

Thanks for the answer . swim did his volvin tek with the C5-C6 NPS. A lot of it vaporized instantly when poured into the hot base solution which sucked a lot, but on the other hand it was easy to evap to get the NPS saturated before freeze precipitation. Swim will try the other half with C6-C7 and posts about the results.

Since there isn't much discoloration (see big as picture - idk why its that tall ) and you say it's not to common to do, swim probably skips it and does only a small scale 100mg one to test how much loss takes place. How much charcoal will be sufficient?(which is a good tip thx)=will update here.

I think DMT oxide is the discoloration right? Wasn't that not really soluble in Naphtha as well?...or is it left over base solution the "blob"? Swim did 3 washes at every pull like in volvins tek...shouldn't it all be gone already?:?:

 

[Bisy]

Yeah, thats right, the original post that I lost included a part about not throwing out the goo blob, that unless you botched your separation pretty bad, it isn't basic soup, and mostly dmt. It does however behave like basic soup contamination, and look like it.. and finally a question: is the goo blob a contributor to the yellow color in crystals? I was assuming that if you repeated the hot nps washes enough, you could eventually have clear crystals. But they wouldn't be close to the amount you started with because most of it was goo blob.

 

[Jules_supertramp]

(STRG is the German keyboard equivalent for CTRL, for those of you who were wondering )
I also find the browser cache (or whatever) keeps my reply window input when navigating back and forth with the ALT+← and ALT+→ keys. Maybe this is not the case for the mobile version?

High(er) BP naphtha can be a very good extraction solvent. Hydrotreated medium naphtha (sold as BBQ lighting fluid but this was 15 years ago) pulled very nicely when warm and gave excellent freeze precipitation results. It would be desirable to follow up an extraction that used high BP stuff whit a re=x or two from light naphtha.

Current thinking is that the brown blob is largely polymerised DMT; at a certain temperature it begins to dissolve. This was very baffling when I first encountered it.

I have Strg as well down there
WTF is polymerized DMT? Sorry but me don't understand :surprised ...like in Ethylen or Propylen polymerization? To create molecule chains?? haven't had chemistry in a while.

And sorry Bisy for that wast of time

 

[downwardsfromzero]

WTF is polymerized DMT? Sorry but me don't understand Surprised ...like in Ethylen or Propylen polymerization?

More or less as you say. The DMT molecules appear to join up into chains of unspecified length but nowhere near as long as your average alkene polymer. Technically, we would say DMT 'oligomers' because it's only a few units joined together. Benzyme did the work on this (iirc). Some of us were discussing it in a thread fairly recently.

is the goo blob a contributor to the yellow color in crystals?

It seems likely that at least some of the yellow coloration is due to the 'goo blob' DMT oligomers. A fairly viable hypothesis would be that electrons are able to move through the interconnected DMT molecules which shifts an energy absorption band into the visible range (i.e from UV to blue/purple, hence the yellow/orange colour).

 

[Jules_supertramp]

Thanks for the answers. So there was no blob all, when swim mixed it with 50ml of 60°C C6-C7:? .
Even tho the crystals where fairly white the liquid turned yellow like piss.

So after SWIM recrystallized there where pretty crystals inside the beaker

but on the bottom it was dark very yellowish brown stuff

. When Swim poured NPS on it, only the withe clear crystals disolved and there was hard dark chunks

left which turned into oil after heating the solvent and sticked to the bottom

. It did not dissolve in NPS and H20 but in ethanol. Why (if this is "polymerized" DMT) does it dissolve in ethanol? It rises it's pH to 9. It also smelled bad when heated and not like DMT at all.

Is this the notorious "blob"?:?: