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Removing NaCl from harmala xtals after manske? Options
 
bongoman
#1 Posted : 3/18/2019 7:25:57 AM
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I've got some nice harmala extract from syrian rue after basifying my xtals after the manske steps.

But I guess there's a bunch of NaCl in there too after doing 5 x manske steps.

Thoughts on dealing with this potential NaCl contamination?
 

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Th Entity
#2 Posted : 3/18/2019 8:04:15 AM

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Hi!
Im not familiar with harmalas extractions (ive never done or read one extraction tek) im not familiar with "manske step".

1) But it makes sense to me, if you have freebase harmalas with NaCL contamination just place your harmalas in water so the NaCL dissolve and the harmala freebase stays solid and then just filter the solids (harmalas) out and discard the liquid (water/nacl). Then just dry your harmalas and collect.

2) Or if you need the harmalas for changa, just dissolve the harmalas in nonpolar (salt wont dissolve in NPS) filter/carefully decant liquid (NPS/harmalas) add DMT in your preferable ratios, evap over plant material.

p.s. - Wait for other responses from people with experience in harmala extractions, take my word with a grain of salt!

Good Luck and share results! (I would like to know if i helped)
Cya Thumbs up



 
pastanostra
#3 Posted : 3/18/2019 10:27:23 AM

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As entity said, water wash is good without loss (if you let enough time to decant) to rince from different water soluble salts (NaCl, NaOH, Sodium Carbonate) you can look at this , see Remove Excess NaOH, Salts, Etc.

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endlessness
#4 Posted : 3/18/2019 11:27:41 AM

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If you indeed have based and have freebase harmalas, there won't be NaCl salt contamination. The NaCl from the previous step wouldn't be there because you redissolve the harmalas HCl from manske in water, which will also dissolve any excess NaCl. Then when you add NaOH or Na2CO3 to the harmala solution to precipitate the freebase, it will precipitate harmalas but not the dissolved NaCl.

The possible contamination would only be excess Na2CO3 or NaOH if you added the base directly to the harmala solution and didn't mix well and some stayed undissolved on the bottom. If you first make a concentrated solution with the base and then add that to the dissolved harmalas solution, you completely eliminate that possibility.

If you screwed up and you did have some undissolved base there, you could do a quick dilute basic water wash on the harmalas but you can lose a small bit of harmaline with each wash because harmaline freebase is slightly soluble in water .

If what you have is not a base but the result of a manske precipitation (harmalas HCl), then obviously you can't wash it with water because it will simply dissolve it.
 
bongoman
#5 Posted : 3/18/2019 9:42:22 PM
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Definitely based, and got a very sudden precipitation as expected, although had trouble stabilising pH at around 9.8, it was moving up and down after stirring in the NaOH.

Thanks for the helpful suggestions. I've attached a pic after filtering and drying the based precipitate but before any cleanup.
bongoman attached the following image(s):
IMG_3921.jpg (2,009kb) downloaded 52 time(s).
 
downwardsfromzero
#6 Posted : 3/18/2019 11:35:33 PM

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Very unlikely there's any significant amount of NaCl in there. Cleanup could include: dissolve in minimum amount of 3% acetic acid and base again to recover. When carefully titrated the solids would have but minimal sodium acetate contamination, and sodium acetate is somewhat more soluble than sodium chloride.




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blue.magic
#7 Posted : 3/19/2019 6:41:09 PM

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Yes there should not be any significant salt contam.

You can wash the freebase with water and as other said, you can redissolve and re-basify with dilute base slowly - crashing the alkaloids quickly with too much concentrated tea or too concentrated base might cause formation of crumbles that might trap some impurities.

If you want NaCl-free hydrochloride salt, one option is to dissolve free base in alcohol, acidify with hydrochloric acid and evaporate the alcohol. The HCl must of course be food safe.
 
 
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