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MHRB low yield clear goo Options
 
pmvnvx
#1 Posted : 6/6/2020 2:53:58 PM

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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:
 

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null24
#2 Posted : 6/6/2020 4:21:13 PM

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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.
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
pmvnvx
#3 Posted : 6/7/2020 11:53:18 AM

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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
#4 Posted : 6/7/2020 4:22:43 PM

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pmvnvx wrote:
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!
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
 
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