MHRB low yield clear goo

[pmvnvx]

Hi everyone,
I've been lurking for a few years and finally decided to create an account.

I am currently extracting DMT from MHRB however I'm left with very little completely clear goo. I did a re-x and got some crystals but it is so little my mg scale measure 0.000g.

Here is the process that I followed (A/B):

Room temperature: 25°C
100g MHRB (freezed 1 times to try to break plant cells)
3 acid wash with HCl at room temp
Basified to pH 9 with Na2CO3
3 pulls with naphta (EC N° 921-024-6) at 40°C
Attempted a freeze-precipitation, no crystals after 6H at -13°C
Did a full evap, a clear goo appeared
Did a re-X, a few very small white crystals were recovered (mg scale measures 0.000g)

I think the acid wash is were it went wrong, I should have used heat.
What do you think ?

Here are my detailed timestamped notes:

Spoiler

T00H00 - In an Erlenmeyer (A), added 100g ground MHRB, covered with 303g of distilled water and 6g of 23% w/w hydrochloric acid
T00H20 - The solution was filtered into a new Erlenmeyer (B) and the MHRB put back in Erlenmeyer (A)
T00H24 - In Erlenmeyer (A), poured 131g water, 4g HCl
T00H44 - Erlenmeyer (A) was filtered into Erlenmeyer (B), MHRB poured back in Erlenmeyer (A)
T00H50 - In Erlenmeyer (A), poured 104g water, 6g HCl
T01H30 - Erlenmeyer (A) was filtered into Erlenmeyer (B), MHRB poured back in Erlenmeyer (A)
-- I slept --
T17H20 - In Erlenmeyer (B), added 5g of sodium carbonate. pH = 9
T17H52 - Started heating Erlenmeyer (B) to 40°C
T22H13 - Poured 50ml 40°C naphta (EC N° 921-024-6) into Erlenmeyer (B)
T23H02 - Pulled 40ml from Erlenmeyer (B) in crystallizing dish (C), poured 50ml naphta in Erlenmeyer (B)
T23H45 - Pulled 50ml from Erlenmeyer (B) in crystallizing dish (D), poured 50ml naphta in Erlenmeyer (B)
T24H00 - Pulled 50ml from Erlenmeyer (B) in crystallizing dish (E), Crystallizing dish (C) (D) and (E) were put in the freezer (T° = -13°C)
T30H00 - Crystallizing dish (C) (D) and (E) were removed from the freezer, no crystals
T30H25 - Poured the content of crystallizing dish (D) (E) into (C) and started full evap
T32H04 - Crystallizing dish (C), no crystals, a clear goo is present in very small amount
T32H25 - Dissolved the clear goo in a few ml of naphta and put in the freezer
T40H02 - A few (~3-4) very small crystals are present, measured on a mg scale: 0.000g, it smells like DMT

 

[null24]

Don't think you based your solution quite enough rather than failing in the acid stage. At pH 9, you are quite far from the point at which a majority of DMT will migrate into your nps. It is not freebased yet. You want to get it to 12, all the way up. Solution should go very dark when it is based, almost black. I honestly never use any pH meter and just go by the color change.

If i've read your process correctly, you should simply be able to raise the pH and pull again to recover your alks. Of course, this is assuming that you are working with actual mhrb and did not acess "bunk bark". That is doubtful though, try raising your pH value.

 

[pmvnvx]

You were right, I raised the pH to around 11 and got some crystals. The solution went from a dark-ish gray to almost black.
I would like to raise the pH to >12 but I'm stuck with Na2CO3 for now.
I'll keep the erlenmeyer until I can have my hands on NaOH.

Thanks for your help.

 

[null24]

You were right, I raised the pH to around 11 and got some crystals. The solution went from a dark-ish gray to almost black.
I would like to raise the pH to >12 but I'm stuck with Na2CO3 for now.
I'll keep the erlenmeyer until I can have my hands on NaOH.

Thanks for your help.

Awesome!