Unexpected occurrences with q21q21 tek

[Levanah]

Hello fellow consciousness explorers!

I'm in the middle of an extraction of 250g MHRB using the q21q21 tek which I have used successfully before - I mastered it and can't explain the unexpeteced occurences in this extraction.

I always salt the d-limonene with pure 5% acetic solution.

I always evaporate the dmt containing acetic solution to retrieve a brownish honey-like full-spectrum dmt-acetate goo. I like to work with that!

Normally my yields match the expected yield.

This time two things went totally different although I did everything as usual:

1. My d-limonene went dark brown (even after salting and letting it sit in the fridge for 24h - the jar on the right side)

2. The yield of my first pull gave 6g waxy stuff. I would have expected at most 1g 99% DMT containing brown honey like full spectrum goo.

So why did the d-limonene go brown this time? And why is my yield possibly contaminated with impurities? What could it be? Base-plant emulsions?

I'm thankful for any advice!

 

[Levanah]

Update: I just bioassayed the material and I suspect it contains at least 12% or moar DMT. Works perfectly fine with my ROA.

It is completely water soluble, so I guess plant-oils or plant-base residues are out of question?

What could be the other 80% then?

 

[Levanah]

Another picture from one of my last pulls.

Looks like it forms three layers:

1. limonene/oil
2. ???
3. vinegar

 

[Hyper Turtle]

I'm pretty sure the 'third layer' in between is just an emulsion.

If it won't separate on it's own, i find a sep funnel useful for that - emulsion separates in the narrowest part at the bottom, frees up a little vinegar, let that off, repeat..
Pouring the emulsion through a coffee filter can also help as a last resort.

Idk why you'd get such a big emulsion, maybe because of the mystery contaminant.

 

[Levanah]

I'm pretty sure the 'third layer' in between is just an emulsion.

If it won't separate on it's own, i find a sep funnel useful for that - emulsion separates in the narrowest part at the bottom, frees up a little vinegar, let that off, repeat..
Pouring the emulsion through a coffee filter can also help as a last resort.

Idk why you'd get such a big emulsion, maybe because of the mystery contaminant.

Thanks for your advice!

I've decided put the glas jar in the freezer and will discard everything which will not freeze, evap the frozen liquid and get my final yield.

I've filtered my dissolved waxy yield through a 0,22um micron filter and got a clear solution (though it was already clear before filtering).

When I add the filtered clear solution into more water to dilute it it becomes a bit cloudy though and looks like a finely micronized water oil emulsion. The "mystery contaminant" seems to be plant oil which is fully soluble in water.

As I couldn't get hands on fresh foodgrade 99% d-limonene this time I had to dilute it with 95% tech grade d-limonene which is almost transparent and doesn't smell like orange but like lemon. Last time (years ago) it worked perfectly with that citrus limonene but now it seems like the 95% d-limonene is the mysterious variable here that messed things up.

Although the spice is good and active, next time I plan to work with medical petroleum ether (naphta) again to yield a moar pure product.

Alchemists say that the spirit of the plant is contained in the oil, the mind of the plant in the alkaloids and the body in the inorganic plant matter. So a little bit more oil it the yield doesn't have to be bad - it has just moar plant spirit in it

 

[Dirty T]

Pour non-Iodized table salt in it and apply heat with a hot pot of water (just use something to keep the jar from touching the pot or boil the water first then turn off the stove and add the jar) and the emulsion will break. I use 60g salt per 50g bark used and never have an emulsion lasting more than 5 minutes.

 

[downwardsfromzero]

As I couldn't get hands on fresh foodgrade 99% d-limonene this time I had to dilute it with 95% tech grade d-limonene which is almost transparent and doesn't smell like orange but like lemon. Last time (years ago) it worked perfectly with that citrus limonene but now it seems like the 95% d-limonene is the mysterious variable here that messed things up.

Looks like this answers the question I would have had. I suspect that the lemon-scented material contains additional oxygenated terpenoids which both contribute to the aroma and react with strong base to produce the dark discoloration that you observed.

It's possible that some of these compounds have a slight detergent effect which will likely have been the cause of the emulsion as well. Furthermore, this brown gunk increases the viscosity of the limonene which in turn increases its tendency to pull bark microparticles onto the polar/nonpolar liquid interface, again boosting the likelihood of emulsions.

It may be informative to test a sample each of your batches of limonene with concentrated sodium hydroxide solution. Then you can be a little more sure about possible contaminants - although limonene itself does slowly oxidise as well, meaning that an older sample will likely show some discoloration even if it was pure to start with.

 

[Levanah]

Thank you guys for your help and advice!

Pour non-Iodized table salt in it and apply heat with a hot pot of water (just use something to keep the jar from touching the pot or boil the water first then turn off the stove and add the jar) and the emulsion will break. I use 60g salt per 50g bark used and never have an emulsion lasting more than 5 minutes.

If I understand it correctly, after adding the table salt and apply heat the emulsion/bark microparticles/whatever will sink to the ground?

And the vinegar/non-polar liquid will then contain dmt acetate and table salt contamination?

When you say "I use 60g salt per 50g bark used and never have an emulsion lasting more than 5 minutes." it reads like your adding table salt before adding the non-polar solvent to the bark mush when you are still in the middle of the extraction. But maybe I get this wrong and you are not even using q21q21 tek.

As I couldn't get hands on fresh foodgrade 99% d-limonene this time I had to dilute it with 95% tech grade d-limonene which is almost transparent and doesn't smell like orange but like lemon. Last time (years ago) it worked perfectly with that citrus limonene but now it seems like the 95% d-limonene is the mysterious variable here that messed things up.

Looks like this answers the question I would have had. I suspect that the lemon-scented material contains additional oxygenated terpenoids which both contribute to the aroma and react with strong base to produce the dark discoloration that you observed.

It's possible that some of these compounds have a slight detergent effect which will likely have been the cause of the emulsion as well. Furthermore, this brown gunk increases the viscosity of the limonene which in turn increases its tendency to pull bark microparticles onto the polar/nonpolar liquid interface, again boosting the likelihood of emulsions.

It may be informative to test a sample each of your batches of limonene with concentrated sodium hydroxide solution. Then you can be a little more sure about possible contaminants - although limonene itself does slowly oxidise as well, meaning that an older sample will likely show some discoloration even if it was pure to start with.

Great explanation and insights you have given me here!

I always wondered why my d-limonene smelled like lemon. It wasn't one of the limonene products with surfactants, that's for sure. But additional oxygenated terpenoids make sense.

The limonene is about 5-7 years old so oxidation may also play a part. Because I have done an extraction with the exact same techgrade limonene before and didn't have these issues.

 

[Levanah]

For the purpose of science and to determine the DMT content of the waxy product I did two experiments:


Experiment 1 (Picture 1):

1. Dissolved 2g waxy product in 1ml water (again, this stuff is fully water-soluble without any signs of a visible emulsion - though dissolving takes some time/30-60min).
2. Added sodium carbonate to the solution, made a paste and let it dry.

I will now do pulls with naptha, though it's very waxy and I'm not sure if it's a 'good to pull from' starting material.


Experiment 2 (Picture 2 and 3):

1. I dissolved 2g waxy product in 2ml water.
2. I added 20ml of a super-saturated sodium carbonate solution to it.
3. I put it in the fridge overnight.

In the morning the 22ml water in the glas jar were "like frozen". I think the sodium carbonate fully crashed out and there were no signs of water anymore.

4. So I added some more warm water and put it in the fridge again

Now I have crashed out sodium carbonate and hopefuly dmt freebase in the bottom from which I can pull.

What are the brown drops? Seems to me like oil that is not behaving like a real non-polar liquid and only crashes out as oil in a super-saturated salt solution?

However, with luck experiment 2 was successfully in seperating the "contaminant oil". I will see later what the freebase yield will look like.

I'll do multiple small 20ml naptha pulls from each of the experiments and theoretically the spirit molecule freebase should be retrieved without significant loss.