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5-10% Ammonia: good enough for harmaloid purification? Options
 
bringeroflight
#1 Posted : 10/25/2010 7:53:35 PM
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swim's doing the manske tek on some rue seeds. The only ammonia that is available to him is not pure, it is a water solution of 5-10% ammonia with nothing else added. Will this work for the tek? Or does it need to be pure? And if it needs to be pure, then what other options might be available to swim, besides ammonia, for further purifying his loids after the salt precip? Thanks.
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endlessness
#2 Posted : 10/25/2010 8:20:55 PM

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Ok first a little comment, manske is the name for the salt precipitation step, therefore for a manske you dont need a base. But if you are doing a harmala extraction (like this) that includes a manske step in the beginning and later uses a base, then yes, that is more than enough.. Youre only gonna need a few drops of that.

Do note that ammonia stinks very much (and it hurts to smell it), please dont work with it indoors unless you have really good ventilation.

Why dont you just use sodium carbonate? You can make it from sodium bicarbonate (which you can buy pure in pharmacies or even supermarkets)
 
bringeroflight
#3 Posted : 10/25/2010 8:28:53 PM
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Great. Thanks endlessness, for the clarifications and advice. If it's unnecessary to go the ammonia route, swim will just use sodium carbonate instead.. sounds a whole lot more pleasant than permeating swim's house with a horrible ammonia smell.

Swim also noticed that another option is to redissolve the loids in methanol, and then evaporate that. Sounds easy enough.. but would the base route be more efficient?
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endlessness
#4 Posted : 10/25/2010 8:38:43 PM

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where did you 'notice this option' ?

you just cant compare using a base to precipitate freebase alkaloids from a solution, and redissolving dry salt alkaloids in a solvent and evaporating, these are completely different processes, so I dont understand what you mean (and I hope you read more if you dont see why they are so different)

Also, there is still some controversy regarding dissolving harmalas in alcohols because an unknown product called Harmala Red can form, and we still dont know what it is and whether its active or not.. Just check the link I sent you for the way to purify.. Do know that filtering will be a pain in the ass one way or another. Just be patient and do with multiple filters at once, leave it filtering and forget about it. Or use a vacuum filtration system
 
bringeroflight
#5 Posted : 10/25/2010 8:53:00 PM
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I noticed it right here: https://wiki.dmt-nexus.m...rystals_from_Syrian_Rue

Sorry, but all of this information is new to me and a lot of what's basic to you I don't even know yet. I haven't had any chemistry training and I'm just trying to piece things together from the reading I've managed to do so far. Sorry if it doesn't make any sense, but this isn't stuff I was born knowing. Please bear with me.

Thanks for all the info.
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endlessness
#6 Posted : 10/25/2010 9:00:46 PM

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Sorry if I sounded arrogant. I wasnt born knowing either Pleased

Check out the link I posted before, the other tek for harmala extraction. Redissolving in methanol as explained in the link you posted may or may not be problematic, but in any case its a very different process than the freebase precipitation. When you do the manske salt precipitation, you precipitate harmalas in salt form (more specifically, Harmine and Harmaline HCl). This means they have an HCl ion attached to it. When you redissolve that in warm water and add a base like sodium carb or ammonia, the raise of the pH will make the Harmalas precipitate in freebase form (without the ion attached). They will be purer because the manske precipitation is very crude, it has a lot of salt and other plant contamination. The freebase is cleaner. Each time you redissolve and reprecipitate, it will get cleaner (Again, read the guide I linked you).

Check the FAQ and the WIKI in general, there is a LOT of information which will make you udnerstand what is going on.. Its definitely recommended that you dont just follow teks but understand why each step is being done.

Good luck and if there's anything else you cant find answers to in your information search, do post Smile
 
bringeroflight
#7 Posted : 10/25/2010 9:04:30 PM
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Okay, thank you once again for helping me understand! This website truly is an incredible resource and you guys are doing a spectacular job making all this knowledge available.

Before continuing to post with questions, I'll take a further look in to the wiki. Thanks for your help!!
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Crystalito
#8 Posted : 10/26/2010 1:55:10 AM
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Personally i have used ammonia 10%,can be found in pharmacies and its pure ammonia if you keep your eyes peeled for ammonia wityh no extra ingredients. Due to the amount of precipitation i used lots of it , basically i used it to redissolve the precipitant (in the hundrends of mls). Looks like it has worked so far. I chose it mostly because it evaporates clean so less contaminants in the final product (well, trying to minimise even minimal sodium carbonate one would have with the other base).

FOr Skullhuman: the basing , either way, will make alkaloids precipitate in freebase form whereas the water will still hold in solution previous contaminants like salt used in manske.

By the way skullhuman what quantities of rue did you use?

An idea: Is freebase soluble in alcohol? If it isnt then one could dissolve the manske precipitate int alcohol (does NOT dissolve salts like NaCl), filter the insolubles out, basify the alcohol and that should precipitate the harmalas. I wonder if alcohol can pull out different impurities that water can pull and if it would make a difference.
 
 
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