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Getting rid of excess salt?? Options
 
Eranik
#1 Posted : 10/29/2010 8:04:14 PM

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How can one get rid of excess salt from harmala HCL?

SWIM likes to boil ground rue seeds, filter, then supersaturate the hot solution with table salt until no more can be added, then put it in fridge, and crystals fall on the bottom.

This way SWIM can be sure she's trapping all of harmala alks, but also with lots of excess NaCl. How to separate the excess table salt?
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endlessness
#2 Posted : 10/29/2010 8:46:06 PM

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I havent found a method for this yet, but what is the problem with salt contamination? The only problem I see is having an unnacurate dosage, but thats easy to solve. Redissolve in water, precipitate the freebase, dry, weight it.. This will be much more accurate weight. If you want it in salt form, measure an exact dosage (lets say, 1g or whatever) redissolve in vinegar, precipitate with excess salt, and divide whatever final product you have in the according number of dosages judging by your original freebase weight.
 
Eranik
#3 Posted : 10/31/2010 3:39:03 PM

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endlessness wrote:
I havent found a method for this yet, but what is the problem with salt contamination? The only problem I see is having an unnacurate dosage, but thats easy to solve. Redissolve in water, precipitate the freebase, dry, weight it.. This will be much more accurate weight. If you want it in salt form, measure an exact dosage (lets say, 1g or whatever) redissolve in vinegar, precipitate with excess salt, and divide whatever final product you have in the according number of dosages judging by your original freebase weight.

How about this, will this work?:

Add some lye to some water to make a high pH water
pour it over what you got (harmal alks and excess salt)
harmal alks will go freebase
add some NPS to dissolve freebase harmal alks
keep the solvent and discard the rest
let the solvent evap
pure freebase harmal alks, keep as is or turn to salt (how?)


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endlessness
#4 Posted : 10/31/2010 3:58:17 PM

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but what have you solved doing this? First of all you have the difficulty of finding a non polar where harmalas dissolve well, which I dont know any. Also, from experience with other alkaloids, I would say its much better to first dissolve the salted alkaloids in the water and then add the alkaloids. Adding them to basic water might work in turning them freebase but it might also form some kind of clathrate-like compound, where there is an external layer that protects the inside from dissolving. I've seen this happen with bufotenine, where it became a sticky gum-like substance instead of mixing properly, I dont know if the same would happen with harmalas.

And then you still have to answer: what would be the advantage of using lye instead of raising the pH with something safer (and equally effective in this case) like sodium carbonate? Also, lets say even if this work, why using a solvent and not simply precipitating it as freebase and filtering, no need to add solvent?

and again you have the same issue with turning it into a salt. You can do as I said before and have some salt contamination but at least know exactly how much of salt contamination to do an accurate dosaging. Another option might be redissolving the freebase in molar-calculated quantities of FASW and evap that, to yield harmaline/mine fumarates (But Ive never done this, just speaking theoretically)
 
Eranik
#5 Posted : 10/31/2010 4:06:27 PM

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I exactly didn't understand what you mentioned about calculating the NaCl to help in accurate dosing, SWIM has lots of salt contaminated alks, how to calculate the salt? what do you mean by redissolve in water and "precipitate the freebase", I don't get this clear.
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endlessness
#6 Posted : 10/31/2010 4:16:20 PM

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Your harmalas are in salt form, therefore they are water soluble. Use some warm water to redissolve it all. The salt contamination will also redissolve. Then you slowly add small amounts of sodium carbonate saturated water. This will make the color change, which is the freebase harmalas precipitating. Add sodium carb solution till it stops changing color (and a bit more just to be sure), and stick in the fridge for some hours. The freebase harmalas are free of salt contamination (because salt remains in solution, doesnt precipitate). Filter, dry, weight. Then you know more accurately how much harmalas you have.

If you want it as salt, knowing the accurate weight of freebase beforehand, you can try redissolving in FASW as I explained in last post and evap that (never done but guess it works), or redissolving in vinegar and re-precipitating with salt, manske-style. Then you'll have some salt contamination again but you know the exact original weight of freebase so you can divide in according number of doses.

also check this guide, it explains the extraction more in-depth:

https://wiki.dmt-nexus.m...ion_and_Separation_Guide
 
Eranik
#7 Posted : 10/31/2010 4:28:38 PM

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Thanks, new light bulbs arise up my head now.

If >> one does get nearly all of harmal alks in freebase form after your process, then is it possible to:
turn them to salt this way:
calculate the exact amount of citric acid needed to turn all the freebase alks into salt,
measure the said amount of citric acid powder
dissolve in methanol
add freebase alks to acidic alcoholic solution
let evap
pure I-don't-know-what (citrate?) harmal salts

Is this possible at all?
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