I took 50 g MHRB and acidified with 4 mL 30% HCl in H2O and 500 mL dH2O. The pH read around 2. This was heated for a little bit but I realized my heating pad was too variable so I just let it soak for a week. After the week it was twice filtered and basified with a solution 3 g NaOH in 7 mL water which caused the color to change from Reddish/Brown->Grey->Oily/Inky Black. The pH read around 13. 50 mL of Naptha was added and the solution was shaken. The emulsion settled within 6 hours and after 24 hours the Naptha was pipetted into a pan which was stuck in the freezer for 12 hours. After those 12 hours, nadda, nothing, zip.
What went wrong? What can I do to fix it?
My thoughts would be to much acid, or too little base.
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Could be that you used way to much naptha and too few pulls? I use say about .5ml naptha/ gram bark, and I do say 4 pulls, il also evap the naptha down till it gets cloudy when blown on. It makes it easier for the DMT to crash out when the naptha is saturated.
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I was going to do more pulls, but just wanted to see how the amount of DMT per pull changed.
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It sounds like your naptha wasn't saturated enough to precip. One should do multiple agitations with thier NP. Could be the lack of heat in the acid soak too - I've never tried a CWE with HCl, but phosphoric CWE's yield significantly lower than when the solution is cooked.
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