Film in naptha

[intechgration]

SWIM started an STB on ~60g MHRB powder earlier this week. He put ~60g MHRB powder in 1.5L distilled H2O with ~200g NaOH dissolved in it. After mixing thoroughly it was allowed to sit for about 12 hours mixing every few hours. 40mL naptha was added, and left in the jar for approx 12 hrs with inversion every few hours. This first pull was put in the freezer at 0 degrees C. The precipitated crystals weighed about 50mg. The naptha was saved and used in a second pull. A third identical pull was performed. After only minimal crystal formation during freeze precipitation, the 2nd and 3rd pulls were combined and completely evaporated, yielding approx 100mgs of crystals.

SWIM assumed that low yield meant that more soaking was needed, and that minimal crystal formation during freeze precip meant that the amount of naptha per pull should be reduced.

20mL fresh naptha were added to the jar and let sit for approx 24hrs with inversion every hour or so, making sure to agitate settled material. Polar and Non-polar layer separated well every time. After the first twelve hours, SWIM noticed lighter colored specks appearing amongst the settled material in the bottom of the jar, and beige-ish pieces of film collecting along the interface of the polar and non-polar phases. When the naptha was pulled out of the jar, care was taken to avoid any of this film. Only a couple hours after placing this pull in the freezer, it had the most crystal formation of any of the pulls yet performed on this extraction. However, after several more hours, a yellowish/beige-ish film formed on the surface of the naptha (looked like the film in the jar, just a bit more yellow), and after several more hours, this film settled upon the crystals.

SWIM is wondering:
1. Are the lighter specks in the settled material, the film at the phase interface, and the film in the freeze precip just fats? If so, was it released by prolonged soaking in the basic solution? If not, then what is it?
2. Will a recrystallization remove this residue?

EDIT: whoops, this should probably be in the General Extractions Help, sorry!

 

[mumbles]

1. Yes they are probably fats. STB brings over a lot of crap that an a/b doesn't
2. Of course. Remember to dissolve in warm naptha and then evap down until cloudy with a fan and put into a freezer for at least 36hrs, 48hrs is better. You want all the spice back yeah? =p

 

[soulfood]

What I think has happened hear is you have too much water with too much lye. You could have gotten away with halfing both these amounts for that amount of bark.

With too much lye, all the bark components break down quite quickly and I imagine if you keep pulling, eventually the naphtha will go quite orange, then dark red, then eventually you won't be able to tell the difference between the solvent layer and the soup because of all the oil and dye in the solvent.

Also because of the excess water a LOT more pulls will be needed to exaust the bark, as the soup will have quite a low concerntration per ml of DMT.

Have you tried doing some heated pulls and shaking the hell out of the mix? Like really shaking it? I imagine with that much lye, an emulsion will not form. Also maybe try a little more naphtha per pull. I'd use about 50ml.

I also recommend using the sodium carbonate wash after this process when using an STB.

Then if you want clean spice a recrystalisation is essential.