Depolymerising DMT? (Rescuing a batch)

[nitrogenaztec]

Hi everyone,

I have a bottle of solution lying stored waiting for me to work on it. I think it has been 2 months... since I made it.

It contains NaOH, mimosa bark, salt, some naptha (hexane actually), and water.

I heard that over time, the NaOH will break down the DMT. But others have said it will store for a long time.

I did get some DMT yield from this, but I got a lower-yield than I expected, probably due to DMT polymerisation. Perhaps I just wasn't quick enough. I'm assuming that is the problem, I allowed too much time for the NaOH to contact the DMT. Annoying but hopefully I can fix this.

I have got some strong HCl solution. I know it is dangerous stuff... I'll be wearing goggles and gloves.

How would I depolymerise my DMT solution? And how would I extract it after? Here is my guess:

1) Add HCl until it becomes slightly acidic
2) Shake and mix and wait until it is depolymiserised
3) Add more naptha and NaOH, and very quickly do the extractions.

OK... so this is a very bad guide because it is missing some details:
1) What pH much is needed? and how to detect it?
2) How long to wait for depolymerisation? How can I detect it?
3) What basic-pH should I aim for, before the extraction? Again, how to detect it.

I don't know how much NaOH is in my solution bottle... I did at the time I made it, but I don't anymore.

TL;DR

I just wanna use my HCl to depolymerise my extraction-mix and not sure how to do it.

 

[Loveall]

Per Mindlusion as soon as the dmt is dissolved, it is broken into individual molecules and aggregation reset. This is because the dissolution energy is much stronger than the more subtle aggregation energy.

Slightly acidic water/pH should do a good job at this. Hot naphtha too.

And, possibly yes, a long time is a concentrated base could agregate DMT, but the reset should be simple after an acid step.

Still, even after reset, the mechanics of xtalization are important and "unwanted" aggregation (oils or orange colors) can re-occur during the naphtha freeze step. To minimize aggregation and maximize uniform xtals in naphtha, slowly lower the temperature, minimize vibratios (e.g. not opening the freezer door), and try to use a seed xtal. Alternatively, slow full naptha evaporation can form good xtals.

I think there are several different factors to consider all at once to make sense of things.

If I'm wrong or misunderstood mindlusion someone please let me know. Cheers.

 

[nitrogenaztec]

Per Mindlusion as soon as the dmt is dissolved, it is broken into individual molecules and aggregation reset. This is because the dissolution energy is much stronger than the more subtle aggregation energy.

Slightly acidic water/pH should do a good job at this. Hot naphtha too.

And, possibly yes, a long time is a concentrated base could agregate DMT, but the reset should be simple after an acid step.

Hi thanks...

I'm more concerned about how to depolymerise the DMT in the solution than in the crystalisation phase right now.

So... OK lets see.... how would I do this? Acidify it? How much? How do I know when it is acidic enough?

Once it is acidic enough... what should I do? Rebasify it? How basic?

 

[Loveall]

Per Mindlusion as soon as the dmt is dissolved, it is broken into individual molecules and aggregation reset. This is because the dissolution energy is much stronger than the more subtle aggregation energy.

Slightly acidic water/pH should do a good job at this. Hot naphtha too.

And, possibly yes, a long time is a concentrated base could agregate DMT, but the reset should be simple after an acid step.

Hi thanks...

I'm more concerned about how to depolymerise the DMT in the solution than in the crystalisation phase right now.

So... OK lets see.... how would I do this? Acidify it? How much? How do I know when it is acidic enough?

Once it is acidic enough... what should I do? Rebasify it? How basic?

I don't know for sure. From experience an acid step alone resets the DMT. For a while it seemed that the details of the step mattered, but that could have been xtalization noise later on from the solvent step. Per mindlusion, an acid step easily resets the DMT and breaks up any aggregation.

After that don't, concentrate the DMT/aquarius base too much. Cyb's max ion Tek is a good guideline. A quart of liquid is used for 2-3g of DMT and pH is not higher than 12. These dilute conditions seem to work well. Then, pull and xtalize carefully (slow temp reduction staring with warm naphtha but not too hot, no vibrations when settling in the solvent, adding a seed xtal). Adding the lye after the naphtha is present minimizes chances of DMT aggregating when it is not very soluble in alkaline water, as the free base DMT migrates not allowing the water concentration to be high.

Taking care of the needs for each step (the best we know how) maximizes chances of uniform xtals. I could be ommiting important steps. For example, the solvent could matter and there are indications that lower molecular hydrocarbons (e.g. lighter fluid) could make it easier to xtalize uniformly than higher ones (e.g. painter's naphtha).

Experiments show that xtalization can be variable and not trivial to control. Even trying to keep everything the same you may see different results from one batch to another.

 

[downwardsfromzero]

One more thing is that adding acid and then base will only increase the volume of liquid. It may help to take into account whether or not this will be helpful.

If you have to, it's probably best to reduce the volume of a neutral solution, acidic only if you can ventilate the fumes (in the case of HCl, at least) and basic solutions absolutely the least of all.

 

[Loveall]

One more thing, Na+ and maybe more so K+ ions can disrupt aggregation forces in the basic water when dmt has poor solubility (again, at high solubility aggregation cannot occur).

To keep the pH gentle and introduce these ions use a salt such as NaCl or KCl.

However, a big excess of ions many can lower the free water activityz reducing the already poor dmt solubility, and pushing dmt for aggregation. There is a balance/optimal amount. Against the max ion Tek is a good reference (~7% NaCl target).

So to summarize the theory:

- DMT xtalization is a complex process. Multiple xtal forms exist. Uniform xtalization is more likely during slow controlled conditions (slow temp reduction of solvent or slow evaporation of solvent).
- DMT can also aggregate (aka "polymerize", oligomerize). This results in non-xtaline arrangements that are waxy, have orange colors, and can even be gooey. It is easy to get this form, simply melt xtals with heat and cool.
- After basing DMT has poor water solubility and can begin to aggregate. It can also do so during the solvent phase, and even after xtalization (if melted and cooled).
- Multiple things can affect DMT aggregation. The max ion Tek parameters are a good reference:

Acid step:
- Details don't seem to matter. DMT easily de-aggregates.

Basing step:
-- 7% NaCl (max ion reference)
-- pH~12 (max ion reference)
-- DMT concentration in water ~0.3% (max ion reference)
-- Solvent present when basing?

Solvent step:
-- Lower molecular weight hydrocarbon could be better (slower xtalization?)
-- Naphtha not too concentrated? (~1% concentration max ion reference). Higher concentration can be OK. If slowly dropping the temp this condition may not be as important.
-- Slow temperature drop with minimal mechanical disturbances). Alternatively if starting with cleaned up DMT, slow evaporation.
-- Similar to the acid step, aggregation can be reset by making DMT more soluble (very high temp). However, only do this away from the plant matter as hot naphtha can pickup more plant impurities.

So there are a lot of factors and some interact. I'm sure some factors are missing too. Others may not be that important. That is why experiments should guide the way and assumptions used only as a starting point ready to be disproved.

When vaping, the dmt form does not matter for raw flame. For more sensitive dialed in electronic devices it can matter since the melting point changes with DMT form (xtals need less heat than goo).