A/B lime/vinegar troubleshooting

[lexhr]

Hey guys,
glad to join, first extraction..

Did a vinegar / lime A/B tek a couple of times with same results.

50g mhrb - blended the damn out of it, to fine powder
Acidification
50ml vinegar, 50ml hot water - mixing, checked ph (under 4) all good
Base
added 50g lime, a little water, mixing checked ph (under 12) -- added 15g more, checked ph (over 12) all good
Pull
added 100ml naptha, warmed the glass container with the base in a crock pot, stired, a good 20min passed etc
looked nice as should - transfered to precipitation jar, stuck it in the freezer.

After a 4-5 hours checked initial results and its not cristals it looks like white blobby substance.
later went to remove naphta, left glass container to vent (0-10 degrees celcius on closed balcony)and the white stuff evaporated also.. not dmt i guess

I did this 4-5 times, getting the same results every time. any idea for troubleshooting?
Does anyone know what the white stuff is then?
Photo attached and here of result in naphta

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[m4estr0]

I don't know what the white stuff is, but here are some things you can improve:

I guess if the MHRB is powdered, a single 'acid' soak suffices. Let it sit for a while to be sure. How long? I don't know! Let's say at least 1 hour.

Did you filter the MHRB before adding the base? Better to do a second and third acid pull then, because a lot of water (and DMT acetate dissolved in it) remains in the MHRB.

The solubility of lime (Ca(OH)2) is only 1.72g/L in water at 20C. Most of the lime you added will not dissolve.

I guess pH >12 is good for A/B with filtering, but higher is better (I would aim at 13). You'll need a stronger base for this, like NaOH or KOH (wear eye and skin protection!)

I would only use 50 mL naphtha pulls with 50g bark. Your naphtha needs to be as saturated as possible for freeze precip to work.

Another issue is mixing the naphtha with the basic soup. The DMT at this point is no longer soluble in the water phase, so it will very very slowly sink to the bottom, but the naphtha is on top. If the soup is too thick, the DMT may be even stuck within the basic soup. Just keep this in mind when thinking of a strategy to mix the naphtha with the basic soup.

For freeze precip, a not too wide jar works best.

Check if you're using the right type of naphtha, and also if your lime is of pure enough quality, or just use NaOH or KOH.

Finally: (this is probably not the cause of your problem but I still like to bring it up) Your jar is made of glass, but about the lid? Has it come into contact with the naphtha or lime? Rubber dissolves in NP solvents, aluminum reacts with bases. Ideally get a Teflon stopper.

 

[lexhr]

Thank you m4estr0 for the input

I guess if the MHRB is powdered, a single 'acid' soak suffices. Let it sit for a while to be sure. How long? I don't know! Let's say at least 1 hour.

ok i did this

Did you filter the MHRB before adding the base? Better to do a second and third acid pull then, because a lot of water (and DMT acetate dissolved in it) remains in the MHRB.

can you explain this to me better please?

I guess pH >12 is good for A/B with filtering, but higher is better (I would aim at 13). You'll need a stronger base for this, like NaOH or KOH (wear eye and skin protection!)

it was aprox 13 in the end !

I would only use 50 mL naphtha pulls with 50g bark. Your naphtha needs to be as saturated as possible for freeze precip to work.

this might be the problem.. i will try tomorrow when i take it out of the freezer, if there is no crystals i will use the naptha again, warm it up and let it evaporate 50%?
Naptha and Lime are good quality and high purity
Lid is good also
problem must be the non-saturated naptha i guess
thanks again.

 

[m4estr0]

Did you filter the MHRB before adding the base? Better to do a second and third acid pull then, because a lot of water (and DMT acetate dissolved in it) remains in the MHRB.

can you explain this to me better please?

Traditionally, with an A/B extraction, after the acid soak, the MHRB is separated from the acidic water. During the acid soak, the DMT is converted to a salt, which dissolves in the acidic water. The plant material also absorbs some of this water, and with that water, DMT salts. So some fraction of the DMT remains in the plant material.

Let's say after separation of water from plant material, 50% of the water remains in your (now wet) plant material. (I don't know if this is a realistic number, it is possible to make a good guess by weighing your plant material before and after, and weighing (or measure the volume) of the added water before and after separation from plant material.). Then after the first acid soak, you will have collected 50% of all the DMT that you can possibly extract in your acidic solution. So 50% is in your acidic solution and 50% remains in your (now wet) plant material. To make the calculation easier, let's say you wait before the plant material is dry before doing a 2nd acid soak. Now this time, you will extract 50% of those 50% remaining in the plant material. That means you extract 25% and another 25% of the total amount of DMT is now in your plant material. A 3rd soak will extract 50% * 25% = 12.5%. And so on. If you combine the water from the 3 soaks you get 50% + 25% + 12.5% = 87.5%.

I think in reality, you will get more than 50% with each soak, so you will do much better than 87.5% with 3 soaks.

Now, more recently, there are "A/B" teks that tell you to leave the plant material in your acidic water when basifying. In this case it is not necessary to do multiple acid pulls, IF:
1) The plant material is sufficiently grinded, or:
2) You basify to pH close to 14 such that the plant material is completely broken down by the base
The disadvantage is that you need more base, even if the plant material is grinded, because the base reacts with the plant material also (most of the plant material molecules are acids, like fatty acids, amino acids), and the fact that your basic soup becomes even muddier than it would otherwise. That's why I consider most of these teks to actually be STB teks, and I think the original acid soak can usually be skipped.

So which of these did you do?

 

[m4estr0]

it was aprox 13 in the end !

According to Wikipedia, lime will only get your pH to 12.5, and from there on, refuse to dissolve.

 

[lexhr]

I did not remove the bark from the acidic mixture, and yes it needed more base then predicted!
Now after 18 i have some yield from precipitation of the glass container from the first post, its not much but as i said i will try the next pull with less naptha in order for it to be more saturated and i think it needs to be a little more heated then i did the last time.

will post photos of current pull and next pull for comparison

 

[lexhr]

it was aprox 13 in the end !

According to Wikipedia, lime will only get your pH to 12.5, and from there on, refuse to dissolve.

i have quite good lime 12.8 pH is the exact number

 

[lexhr]

This is first pull.. ( from photo in first post)