newwaveparticle
Rising Star
- Merits
- 42
So I recently performed my first extraction. I followed Marsofold's tek.
Used vinegar as the acid. Mixed 500g pre-powdered mhrb in a crock pot and 1/2 gallon (~2 liters) of distilled water, heated up for about an hour, decanted the very dark red/brown liquid. I repeated with the remaining 1/2 gallon of water by adding 1/4 gallon twice and filtered all the water from the mhrb with a t-shirt. pH was measured at about 3, more towards 2.8 towards the end.
I reduced the ~4 L of liquid to about 700 mL without boiling (~70-80C). Defatted in a 1L sep funnel by adding warm naptha twice (near 100C- is this too hot?).
Added ~200 mL of NaOH saturated water. My pH meter was calibrated around 7 pH and was having issues reading above 13 (I think I would have needed the ~10 pH calibration solution to be very accurate higher- its actually a nice meter). So I added excess lye after reading it wouldn't be harmful.
Put alkaline solution (which was very black, sorta tar-like but watery) in the sep funnel, and performed 5 pulls with 100 mL of naptha each. Naptha was again warmed to about 100 C for each pull. Each pull was around 5 minutes. That might have been too short? I spun it around slowly, end over end etc.
Performed a calcium carbonate wash with very near saturated calcium carbonate/water solution followed by cold distilled water. Let it all separate very quickly and removed each time.
Lastly, evaporated some of the naptha, freeze precipitated. Left me with a bit of white/yellow crystals after I scraped out the jar. I didn't have a scale, but it was probably closer to 1 g or so (still not impressive!).
Recrystallized with heptane/bestine, I added warm (~55 C) bestine with an eye dropper. I only had to add a very tiny amount to dissolve all the white crystals leaving a layer of dark yellow oil and clear bestine on top. I sucked off the oil and put most of it back in the naptha. The heptane was free precipitated and poured off leaving 120 mg of white crystals.
Where did I go wrong?
Point's I think it may have been- naptha pulls- not long enough? Too hot?
recrystallization- too little heptane? Some tek stated ~15 mL of bestine per gram of crystal, I'm sure I added far less but it all dissolved still.
Quality of mhrb? I bought it from a vendor on bonanza. I recently ordered more from KTBotanicals having heard its good.
Used vinegar as the acid. Mixed 500g pre-powdered mhrb in a crock pot and 1/2 gallon (~2 liters) of distilled water, heated up for about an hour, decanted the very dark red/brown liquid. I repeated with the remaining 1/2 gallon of water by adding 1/4 gallon twice and filtered all the water from the mhrb with a t-shirt. pH was measured at about 3, more towards 2.8 towards the end.
I reduced the ~4 L of liquid to about 700 mL without boiling (~70-80C). Defatted in a 1L sep funnel by adding warm naptha twice (near 100C- is this too hot?).
Added ~200 mL of NaOH saturated water. My pH meter was calibrated around 7 pH and was having issues reading above 13 (I think I would have needed the ~10 pH calibration solution to be very accurate higher- its actually a nice meter). So I added excess lye after reading it wouldn't be harmful.
Put alkaline solution (which was very black, sorta tar-like but watery) in the sep funnel, and performed 5 pulls with 100 mL of naptha each. Naptha was again warmed to about 100 C for each pull. Each pull was around 5 minutes. That might have been too short? I spun it around slowly, end over end etc.
Performed a calcium carbonate wash with very near saturated calcium carbonate/water solution followed by cold distilled water. Let it all separate very quickly and removed each time.
Lastly, evaporated some of the naptha, freeze precipitated. Left me with a bit of white/yellow crystals after I scraped out the jar. I didn't have a scale, but it was probably closer to 1 g or so (still not impressive!).
Recrystallized with heptane/bestine, I added warm (~55 C) bestine with an eye dropper. I only had to add a very tiny amount to dissolve all the white crystals leaving a layer of dark yellow oil and clear bestine on top. I sucked off the oil and put most of it back in the naptha. The heptane was free precipitated and poured off leaving 120 mg of white crystals.
Where did I go wrong?
Point's I think it may have been- naptha pulls- not long enough? Too hot?
recrystallization- too little heptane? Some tek stated ~15 mL of bestine per gram of crystal, I'm sure I added far less but it all dissolved still.
Quality of mhrb? I bought it from a vendor on bonanza. I recently ordered more from KTBotanicals having heard its good.
