Mini a/b help

[redbird]

Was trying to find how to do a mini a/b and wasn't able to find a good guide on it so decided to wing it. Shortly after things went wrong, found a post that included what might be the missing step that snarfed everything up.
Did not dissolve into nps to start.

Instead, dissolved 1g into 30ml %5 vinegar. Didn't all dissolve initially so soaked in hot water bath and all but some obvious impurities dissolved. Made a solution of 4g lye in 50ml water. Added roughly 30ml of that to the vinegar. Instantly went milky and shortly after precipitated what looked like crashed harmalas except they all floated.
Poured into sep and added 30ml of warmed naphtha. The precipitate diffused among the aq layer but didnt seem to migrate into the nps. Performed a similar roll "shake" as original pulls, twice for roughly 30 rolls each.
Still not migrating, added remainder of base solution thinking that might push it over. Didn't seeem to be getting better so went ahead and drained aq layer which still included a good deal of precip and then put the nps into the freezer. Not sure what to expect there, quite a bit was already "crashed out" even before chilling.

1) is the key mistake not pre-dissolving in nps?
2) is the precip potentially sodium acetate?
3) was the volume i tried to use too small? How mini are we actually talking?
4) should i just combine everything and start over at a larger scale?
5) pH meter wasn't available at the time and will use in the future but i assume the quantities i used would have put the pH where it should have been, maybe in excess. is that not accurate?

 

[Sakkadelic]

Hi @redbird
Dissolving in NPS first is not necessary I don't think that was the problem
So after turning milky and a precipitate floated to the top, did it stay milky? The dmt usually stays suspended and the solution remains milky until depleted by NPS pulls.

 

[redbird]

Appreciate the quick response @Sakkadelic
Not really, it is a bit cloudy but seems as if most everything precipped and floated like the opposite of a harmala extraction.
Are multiple pulls done in a mini ab? I was assuming the 30ml warmed naphtha would pull almost the whole g in one go.

 

[Sakkadelic]

Yeah multiple pulls are usually done.
1g is at the limit of what 30 ml of naphtha can hold

Chemical Guide to classic Psychedelics (DMT, 5-MeO-", Mescaline, Harmalas, Salvinorin A, ...)

This is a Compilation of chemical properties of the Nexus' members most common molecules to come across. Not all are Psychedelics, but some are just other imporant molecules or derivates. People searching the internet for temperatures to evaporate DMT or similar compounds will quickly stumble...

forum.dmt-nexus.me

It may be that the fine dmt particles coalesced and floated due to the high concentration. Try warming the whole solution with naphtha in there. Warmed naphtha cools quickly when in contact with the cold water and vessel.

 

[doubledog]

If your DMT is in oligomer form, solubility in naphtha could be lower, some portion of it maybe won't dissolve at all.

Edit: I am not sure, but oligomer seems to be produced by too alkaline environment, you've probably added to much lye.

 

[Transform]

Going back to nearly the start, if some of it wasn't dissolving in acid (vinegar?), did you try adding more acid? You should be able to calculate whether 1g of DMT will dissolve fully in 30mL of 5% vinegar.

It goes as follows:
Will those 150mg of acetic acid get fully neutralised by 1000mg of DMT?
[determine their respective reaction proportions by using molecular 'weight' (mass)]
MW [CH₃COOH] = 60
MW [C₆H₄{NHCH:C(C₂H₄N(CH₃)₂}] = 188
[these react in a 1:1 ratio]
60g of acetic acid react with 188g of DMT.
[scale down and divide to common factor]
30mg 'a' react with 94mg 'd'
[multiply by 5…]
150mg 'a' react with (only) 470mg 'd'

You'll need more than twice as much vinegar as you first used in order to dissolve 1g of DMT.

Edit: But did anyone check my workings? Ther was an important part missing…
How much acetic aid is there really to be found in 30mL of 5% vinegar?

Vinegar percentages are typically expressed as w/v so 100mL vinegar would contain 5g acetic acid. Therefore 30mL vinegar actually contains 1500mg acetic acid, which is more than enough to dissolve the 1000mg DMT.

Always check your workings, especially if there's a step missing

 

[redbird]

Recapping

1) is the key mistake not pre-dissolving in nps?
-No, appears optional

2) is the precip potentially sodium acetate?
-Unanswered

3) was the volume i tried to use too small? How mini are we actually talking?
-Potentially but not necessarily

4) should i just combine everything and start over at a larger scale?
-Kinda seems like it, though I only have a 100ml sep. First I'll recombine in sep and warm together to observe what happens.

5) pH meter wasn't available at the time and will use in the future but i assume the quantities i used would have put the pH where it should have been, maybe in excess. is that not accurate?
-Seems like it might be the opposite problem. Should have only used roughly 1.5g of NaOH to avoid the excess mentioned by doubledog. Though I'm not sure as I don't know all the formulas like Transform shared.

 

[doubledog]

1) no, that's fine
2) no, precipitate is your desired DMT freebase. If in clean solution, DMT precipitates similarly to harmalas, but do not settle on the bottom, it floats.
3) no, fine volume
4) no, try to dissolve it in multiple pulls with naphtha.
(There is one simple test: try to add toluene instead of naphtha, if it dissolves the precipitate, it was DMT oligomer. Ofc, to get your DMT out of toluene is not so easy, so do this only if you know what to do next.)
5) Maybe even less lye should have been used. NaOH is pretty strong base and you are basifying a small amount of slightly acidic solution without any solid plant material. No much lye needed for that. Better to add small additions of lye.

 

[Sakkadelic]

2) is the precip potentially sodium acetate?
-Unanswered

Unlikely as it should be readily soluble in water.

4) should i just combine everything and start over at a larger scale?
-Kinda seems like it, though I only have a 100ml sep. First I'll recombine in sep and warm together to observe what happens.

Sounds like a good plan.

5) pH meter wasn't available at the time and will use in the future but i assume the quantities i used would have put the pH where it should have been, maybe in excess. is that not accurate?
-Seems like it might be the opposite problem. Should have only used roughly 1.5g of NaOH to avoid the excess mentioned by doubledog. Though I'm not sure as I don't know all the formulas like Transform shared.

With A/B reactions, you can add things slowly and rely on observing changes. For example add lye solution few mls at a time with stirring until the solution turns milkey, add a few more mls for good measure and stop.

 

[doubledog]

fc, to get your DMT out of toluene is not so easy, so do this only if you know what to do next

Obviously, if you work with lab quality toluene, you can simply evaporate it.

 

[Transform]

NaOH is pretty strong base and you are basifying a small amount of slightly acidic solution without any solid plant material. No much lye needed for that

Molar reaction ratio for NaOH with acetic acid is 1:1, mass ratio is the ratio of their respective molecular masses, i.e. 40:60, == 2:3 therefore to fully neutralise 1.5g AA we only need 1g NaOH or, e.g., 5mL of a 20% w/v solution.

 

[redbird]

Molar reaction ratio for NaOH with acetic acid is 1:1, mass ratio is the ratio of their respective molecular masses, i.e. 40:60, == 2:3 therefore to fully neutralise 1.5g AA we only need 1g NaOH or, e.g., 5mL of a 20% w/v solution.

Haha yea i added way too much then.
Goodness.

Thanks everyone. Really appreciate all the help.

I'm gonna recombine and try warming everything. Seems like I probably gooed everything by over basing so looks like I should get another chance to practice the mini a/b after this one is done.

Since I'm using a weak acid, do I need to leave it in the acid phase for a while to clear up the cross-linking or whatever it's called? Been a few weeks since I read the minimum polymer thread so I can't remember.

 

[redbird]

The first two pulls dont seem nearly as gooey as I expected. Some yellowing bits. Debating if I even need to re-do the mini a/b after I finish this one.
If not for purity then maybe just for practice.