A reduction using vinegar and zinc was done on some full spectrum harmalas and was precipitated with sodium carbonate. Ethanol was added twice to try and remove the harmalas and leave the zinc carbonate. After evaporation there was an amount left that appeared to be larger than the amount initially used for the reduction. End result was soaked in alcohol again to see if anything had been picked up that was unwanted. Immeditaly there was a percipitaction at the bottom that appeared white and bumpy in surface texture. Very shortly after there was a percitation that appeared to just be white slurry forming a separate layer on top. Could this have been a zinc carbonate impurity or impurities from the vinegar and alcohol used? The latter are less of a concern, but one would not want to knowingly ingest zinc carbonate.
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Zinc carbonate contaminated THH?
- Thread starter whatlurks
- Start date
The two substances were seperated via decanting. The bumpy crystaline substance that precipitated first may be trash unless told otherwise. Harmalas, one might gather, are at least slightly soliable in alcohol since that is how people make changa. This bottom percipitaction seems to not be soliable at all in room temp alcohol. One might think the slurry that precipitated slower is the harmalas.
Nereus
Rising Star
Your starting full spectrum harmalas,were they salt form when you began working with them,did you perform a manske step?
I'm asking because i tried to re-x with etoh some full spectrum harmala salts and after they dissolved completely there were NaCl contaminations left behind.
I'm asking because i tried to re-x with etoh some full spectrum harmala salts and after they dissolved completely there were NaCl contaminations left behind.
I see. That's likely what it was then. The starting point of this operation was with a freebase powder as opposed to hcl or anything crystalized. After evaporation there was still about 4 grams more than what was started with (5 grams) but it is all the same consistency and has a slightly more red/brown color so it is likely red harmala by-product making the difference at this point.
TreehouseChemist
Lost Soul
So if you started with full spectrum freebase harmalas, and then did the vinegar/zinc reduction and added carbonate you should have a white precipitate which was zinc carbonate and a mixture of harmine and THH (reduced from harmaline). This precipitate should weigh more than the initial mix of harmalas because it also has zinc carbonate in addition to the precipitated harmalas.
I'm not sure exactly what you did after this, but I will tell what I normally do and you can tell me what you did different.
1.Heat or air-dry the precipitated harmalas/zinc carbonate (let's call it Precipitate 1) to drive off any remaining water.
2.Put Precipitate 1 in a flask with USP-grade isopropyl alcohol that has been dried/stored with anyhydrous magnesium sulfate (from baked epsom salts) to remove any water (ethanol should serve the same purpose as long as it is pure and dry).
3.Heat the flask containing Precip 1 and alcohol on hotplate with mag stirring until alcohol is gently boiling.
4.Vacuum filter the alcohol while still hot and place in a clean flask or beaker (I usually rinse or resoak with fresh hot alcohol again to get any remaining harmalas, add to flask, and top with foil to keep vapors from escaping).
5.Discard the remainder of Precipitate 1, and place covered flask with filtered alcohol in freezer overnight or longer.
6.Decant/vacuum filter the alcohol to recover the cleaned harmala precipitate (Precipitate 2). The leftover alcohol will be dark red (if starting from pure harmaline, probably dark reddish brown if using a harmala mixture with harmine).
7.If Precipitate 2 is reddish-colored instead of white, I usually redissolve in hot alcohol and precip again to clean it up (again, not sure how it will look if starting with a mixture of harmine/harmaline).
Once Precipitate 2 is cleaned up to white it is ready to go. I sometimes A/B it if it is still red instead of re-xtalling from alcohol, but I have tried to Manske salt precip pure THH and it does not come out, so I do not use that for cleaning.
My yield (starting with purified harmaline) is usually 30-40% of the starting material. Low, but pure (I also let the zinc/acid reduction bubble for several days to ensure complete conversion. This is probably excessive).
Things that may make your results different from mine:
1. You started with harmine/harmaline instead of pure harmaline. You should (in theory, but I've been up since Friday) have a higher recovery rate because I believe some of the harmaline is lost in the reduction/purification process. Harmine is not reduced by the H2 bubbles (Verified by reducing harmaline with small amounts of harmine in it that was tested by HPTLC, which showed that the harmaline was fully converted but the harmine remained).
2. Your ethanol could be wet/contaminated with another solvent/something else. I don't know if water would affect the results since zinc carbonate is supposed to be insoluble in water, but I have always used dried alcohol. Did you start with sealed lab grade alcohol, 95% grain, vodka, what?
3. Depending on the type of vinegar you used, that could have added weight too (if using cheap grocery store distilled white vinegar it should not add a significant amount of weight).
Regarding the immediate white precip you got from alcohol, harmalas are soluble in room-temp alcohol but only slightly. If it was fully saturated, even a slight jostling or minor alcohol evap could be enough to precip some harmalas. Texture and float/sink doesn't tell much as tiny particles of harmalas can stick to the surface of a liquid and both harmalas and zinc carb are white/white-ish. I can say from experience that zinc carbonate will not dissolve in even boiling isopropyl alcohol no matter how much you add.
I know this post is a bit rambling, but I'm sleep deprived and just trying to include any info that might help. If you can add some details about your process I can write a more concise answer after I get some sleep.
As long as you had clean vinegar/zinc/alcohol, either vacuumed through filter paper or waited a while (6-12 hr?) to make sure the dust was fully settled before decanting, and freeze precipped, you should not have any contam in your final product. But also, your product should weigh LESS than the starting material. If you end up with more weight, you have added something (mostly likely a zinc salt) and need to clean further. Hot alcohol + freeze precip works for separating harmalas from zinc salts. If the product comes out red and/or sticky, try re-xtalling from hot alcohol and/or an A/B precip and it should clean up.
Going to sleep now
-Treehouse
I'm not sure exactly what you did after this, but I will tell what I normally do and you can tell me what you did different.
1.Heat or air-dry the precipitated harmalas/zinc carbonate (let's call it Precipitate 1) to drive off any remaining water.
2.Put Precipitate 1 in a flask with USP-grade isopropyl alcohol that has been dried/stored with anyhydrous magnesium sulfate (from baked epsom salts) to remove any water (ethanol should serve the same purpose as long as it is pure and dry).
3.Heat the flask containing Precip 1 and alcohol on hotplate with mag stirring until alcohol is gently boiling.
4.Vacuum filter the alcohol while still hot and place in a clean flask or beaker (I usually rinse or resoak with fresh hot alcohol again to get any remaining harmalas, add to flask, and top with foil to keep vapors from escaping).
5.Discard the remainder of Precipitate 1, and place covered flask with filtered alcohol in freezer overnight or longer.
6.Decant/vacuum filter the alcohol to recover the cleaned harmala precipitate (Precipitate 2). The leftover alcohol will be dark red (if starting from pure harmaline, probably dark reddish brown if using a harmala mixture with harmine).
7.If Precipitate 2 is reddish-colored instead of white, I usually redissolve in hot alcohol and precip again to clean it up (again, not sure how it will look if starting with a mixture of harmine/harmaline).
Once Precipitate 2 is cleaned up to white it is ready to go. I sometimes A/B it if it is still red instead of re-xtalling from alcohol, but I have tried to Manske salt precip pure THH and it does not come out, so I do not use that for cleaning.
My yield (starting with purified harmaline) is usually 30-40% of the starting material. Low, but pure (I also let the zinc/acid reduction bubble for several days to ensure complete conversion. This is probably excessive).
Things that may make your results different from mine:
1. You started with harmine/harmaline instead of pure harmaline. You should (in theory, but I've been up since Friday) have a higher recovery rate because I believe some of the harmaline is lost in the reduction/purification process. Harmine is not reduced by the H2 bubbles (Verified by reducing harmaline with small amounts of harmine in it that was tested by HPTLC, which showed that the harmaline was fully converted but the harmine remained).
2. Your ethanol could be wet/contaminated with another solvent/something else. I don't know if water would affect the results since zinc carbonate is supposed to be insoluble in water, but I have always used dried alcohol. Did you start with sealed lab grade alcohol, 95% grain, vodka, what?
3. Depending on the type of vinegar you used, that could have added weight too (if using cheap grocery store distilled white vinegar it should not add a significant amount of weight).
Regarding the immediate white precip you got from alcohol, harmalas are soluble in room-temp alcohol but only slightly. If it was fully saturated, even a slight jostling or minor alcohol evap could be enough to precip some harmalas. Texture and float/sink doesn't tell much as tiny particles of harmalas can stick to the surface of a liquid and both harmalas and zinc carb are white/white-ish. I can say from experience that zinc carbonate will not dissolve in even boiling isopropyl alcohol no matter how much you add.
I know this post is a bit rambling, but I'm sleep deprived and just trying to include any info that might help. If you can add some details about your process I can write a more concise answer after I get some sleep.
As long as you had clean vinegar/zinc/alcohol, either vacuumed through filter paper or waited a while (6-12 hr?) to make sure the dust was fully settled before decanting, and freeze precipped, you should not have any contam in your final product. But also, your product should weigh LESS than the starting material. If you end up with more weight, you have added something (mostly likely a zinc salt) and need to clean further. Hot alcohol + freeze precip works for separating harmalas from zinc salts. If the product comes out red and/or sticky, try re-xtalling from hot alcohol and/or an A/B precip and it should clean up.
Going to sleep now
-Treehouse
Thanks for such a thorough reply. The alcohol used was 95% grain. The harmalas did crash out quickly as they are, as you said, only slightly soliable at room temp. However, the mystery percipitaction crashed immediately as if it was not soliable at all at room temp. Cheap white vinegar was used. Also, when getting the harmalas out of the alcohol they were evaporated with a fan as opposed to vacuum filtered. It is understood after further reading this could cause oxidation which some believe to be the cause of harmala red.
However, the mystery percipitaction was discarded as it was most likely zinc carb or sodium carbonate. 20 mg of the red/brown harmalas were smoked as a test and were found to either be quite active and psychedelic on their own or to have interacted strongly with the little residue in a GVG. Similar in intensity in terms of visuals to that of LSA. May be a little less pure now, but the whole experience was far from unpleasant. Not too worried. Being a kitchen chemist limits the ability a little bit, but with error can come experience and knowledge going into future trials.
However, the mystery percipitaction was discarded as it was most likely zinc carb or sodium carbonate. 20 mg of the red/brown harmalas were smoked as a test and were found to either be quite active and psychedelic on their own or to have interacted strongly with the little residue in a GVG. Similar in intensity in terms of visuals to that of LSA. May be a little less pure now, but the whole experience was far from unpleasant. Not too worried. Being a kitchen chemist limits the ability a little bit, but with error can come experience and knowledge going into future trials.