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.