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Harmalas Extraction and Separation Guide Options
 
plumsmooth
#41 Posted : 4/19/2010 10:41:09 PM

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Update... Precipitates appeared slowly and very small in size compared to the lovely Rue Harmala Needles that are usually obtained. These precipitates look to be clearly harmalas; they are even smaller than the freebase Caapi harmalas. Some of them are floating... Much harder to filter too; must be the cold salt slowing things down a bit. Using 102 filter disks. At this point my conclusion is, for whatever unexplained by-me-reason, Manske & Caapi are just not a good match. Although I would prefer to have the salts, I doubt I will try A Manske Caapi again.

However, I may attempt to convert to salt form by dissolving in acidic water and evaporating.

There is a curiosity regarding attempting Caapi Harmaloid Phosphates as a final salt form prior to tincture making or pharma drinking...

Over and Out...
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
RigaCrypto
#42 Posted : 5/31/2010 1:54:16 PM

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How long would this entire operation take for about 25g of Harmala seeds?
 
Deleriant
#43 Posted : 6/1/2010 11:22:45 AM

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Could this tek be used for passiflora incarnata? I've read that there are relatively few useful alkaloids in passiflora incarnata...would there be any point to trying an extract on around 30g?
 
endlessness
#44 Posted : 6/1/2010 12:35:40 PM

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I dont know if you are going to get any significant amount of alkaloids, I can imagine it also depends on the specific genetics of the passiflora plant in terms of alkaloid content. But I think its always worth it to try for the sake of testing and sharing the knowledge to the community! If theres any good yield, great, if not, then at least we know Smile

The same principles of extraction should work, yes. You could even skip the salt saturation part and go straight for the base-precipitation if you want, or you could do it exactly like the guide, both should work. So if you do try, dont forget to let us know how it went!
 
Deleriant
#45 Posted : 6/1/2010 12:50:45 PM

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Mkay, no reason not to I guess. I've already pretty much put it down to a waste of ten bucks, and if it benefits the community then why the hell not? Very happy

I'll get onto it next time I have a kitchen that doesn't also accommodate non-believers at my disposal Razz
 
RigaCrypto
#46 Posted : 6/2/2010 6:03:17 AM

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I've started an extraction using about 18g of Harmala seeds. I've left it in the fridge for about an hour after adding salt, and then I've left it in a coffee filter overnight. There is still a bit of liquid in the filter, and there seems to be a small, barely scrapeable quantity of brown-reddish powder.

The thing is, the entire coffee filter is impregnated with liquid and what look like shimmering crystals (probably the salt). So, if I just scrape it, I was worried whether I might lose a large part of the alkaloids, that could be impregnated in the paper. When re-dissolving them in boiling water with vinegar, I suppose I can just soak the entire coffee filter. But what about when retrieving the final product? Couldn't a sizable portion of the alkaloids remain impregnated in the paper?

If that was a risk, I could try using a plastic funnel with just a small patch of filter paper covering the hole. Or I could just smoke the paper to use the remaining alkaloids.
 
endlessness
#47 Posted : 6/2/2010 9:24:12 AM

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18g of seeds is not much to play with, thats your first problem imo.. its better to extract a sizeable quantity to make it worth it, like at least 50 or 100g.. This way most of the harmalas will be piled up on each other and not spread all over the filter being hard to retrieve.

In any case: yes, there is no need to filter till perfectly dry the first salting step. Redissolve it in boiling water, vinegar is not even necessary because harmala hcl are water soluble as-is. You can soak the filter in boiling water, as you suspected.... If you were redissolving freebase harmalas, then yes vinegar would be necessary apart from hot water.

As for the final product, after you add the base, let it precipitate/crystalize over a day or so, and then filter. A small filter part covering the whole of a funnel sounds like it could be a problem first of all in terms of the water actually passing through the side of the filter, or secondly, the harmalas and impurities clogging the filtering and making it take forever. You can try it, though, just remember to save any filtered liquid in case your harmalas passed through.

Since when I extract I do larger quantities, in relative terms what stays in the filter is only small amounts. So when precipitating the freebase I filter till nearly dry, then slowly scrape with a straight-blade razor the harmalas (without scrapping fibers of the filter out) and put them on a plate to finish drying, and I soak up the filter in some vinegar and hot water to pick up any filter-trapped harmalas. This I store separately for either next time I extract harmalas, or if I am going to repeat the process to clean it up further I put together with the next round.

good luck
 
RigaCrypto
#48 Posted : 6/2/2010 1:31:30 PM

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Thank you Endlessness. I just want some usable harmine for my first oral DMT trip, and I have a small quantity of Rue to work with so I don't want to mess it up. I'm not overly concerned about purity as the only alternative is Rue tea.
 
RigaCrypto
#49 Posted : 6/3/2010 9:06:11 AM

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I've arrived at step sixteen with about 1/2l of yellow-brownish tea to which I added about 2 teaspoons of sodium bicarbonate to precipitate the harmine. However, there was no color change as you said in the tek. Should I add more bicarbonate? I was worried it would not dissolve anymore and I would be unable to separate it from the precipitated harmine.

Also, could it be a problem that the Rue is three years old? Everything I've read said that the plants have a very long shelf life.
 
endlessness
#50 Posted : 6/3/2010 10:42:27 AM

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is there any vinegar in the solution or was it pure salt harmalas redissolved in water? If there was vinegar, this means a lot of the bicarb you use will first be neutralizing the vinegar, and only once all of it is neutralized, it will start changing colour and precipitating. (thats why I preffer no vinegar when redissolving harmala hcl).. But yeah just keep adding sodium bicarb to precipitate harmine.
 
RigaCrypto
#51 Posted : 6/3/2010 12:27:05 PM

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Yes, I've added a dash of vinegar each time when boiling the seeds, as it said in the tek.

I've piled on more bicarbonate, about 35g, whereas I had added at most 5ml of acetic acid in total. It ended up not dissolving so I added a bit more water. Now it's been sitting for about half an hour and there is no precipitate visible. But you said leave it for a day, so I'll see what happens.
 
endlessness
#52 Posted : 6/3/2010 12:33:30 PM

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colour changing should be immediate. Thats why I preffer to alternate between salt and base precipitation, because then when basing the redissolved harmala salts in pure water, there is not this issue of having to first neutralize the vinegar before the harmalas precipitating and neither problems with undissolved base.

What you can do now is either one of these:

1- start adding sodium CARBONATE instead, which is a stronger base and will faster neutralize any vinegar as well as make the harmalas precipitate. You will have a mix of harmine/harmaline and not just harmine (but you can separate it later if wanted)

2- Add more vinegar (to make sure the harmalas are redissolved and not precipitating), saturate with salt and let precipitate the harmala salts, filter, redissolve salt in pure water and THEN precipitate with base


3- try to add some more sodium bicarbonate and see if colour changes. What colour is the liquid now, btw?
 
RigaCrypto
#53 Posted : 6/3/2010 1:19:37 PM

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The liquid is now dark yellow (it is pretty diluted too, 18g of seeds in about 1/2 l of water.

I've added sodium carbonate and there was no color change whatsoever. No precipitation either. I'm beginning to think the seeds were degraded or I've somehow messed it up otherwise. Maybe I didn't leave it enough in the fridge after the salt precipitation, or maybe all the alkaloids remained in the filter paper, even though I boiled the filters in the water? Or maybe I left them too much with the salt and they precipitated in the pot and stayed behind when I decanted the liquid from the excess salt.

Anyways, I'll make some tea out of the remaining seeds and see whether it has any effect.
 
RigaCrypto
#54 Posted : 6/5/2010 6:38:48 AM

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I've managed to score more Rue, against all odds, and I've done another extraction. Now I have some brick-colored powder after the first sodium bicarbonate precipitation. Thank you Endlessness for your advice. It seems that it was just the seeds I tried first that were degraded. Now I used 150g of seeds but the precipitate after saturating with salt was way more than ten times what it was before.

It's also a fun extraction. I feel like a wizard, mixing a potion in a pot on the fire and purifying out the magical essence. Whereas when extracting DMT by STB I just felt like a meth cook, pouring dangerous chemicals in my bathtub.

The downside with the harmala extraction is the duration though. It will probably come to 24h or so just to complete the first base precipitation. If I want to purify further, I might as well grow a wizard's beard until it's ready.
 
endlessness
#55 Posted : 6/5/2010 9:41:09 AM

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lol man awesome you got it done now! Smile

btw, if you do a food-safe limonene extraction with DMT, it totally changes the feeling than when using naphtha...
 
Eden
#56 Posted : 6/28/2010 3:00:51 PM

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I didn't spot any yeild reports, so I will post mine.

From a hasty extract of 100g rue seeds, 7.8g of harms were collected.
This seems quite high, above even the theoretical 7%.

This was with 4 complete filterings of the redissolved harm salts.
 
plumsmooth
#57 Posted : 6/28/2010 8:58:51 PM

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A couple of thoughts/questions...

First, now that I have the Washing Soda variation for precipitating,
I am wondering what the correct order is in terms of Salt/Vinegar precipitation, Freebase with Sodium Bicarbonate etc...?

Which one might be done first, second, and so on to make for the greatest ease in filtering.

For example, freebase Harmaloids seem smaller and harder to filter sometimes.
However, some gunk/stuff that comes through when salting Manske style may stay trapped in solution when Basifying.

SO I was wondering if after the 1ST Manske salting, whether one should go right to a Freebasing, or whether to run the Manske 2 or 3 times first.

And even then, if one is planning on ingesting, then is Basing even necessary or useful toward clean up and a purer product?

Also, Secondly, I'd like to suggest that it is probably good to just stay with the given formula of 100g Salt per 1000ml water.
Why, because for one, more salt doesn't yield any more Harmalas.
And two, because any extra salt just adds to the remaining salt in final product.

Now, especially if proceeding three times or more with the "dissolve as much salt as possible" approach while boiling-- doing it by Eye...
This, In my opinion would definitely lead to excess salt in final product, especially since the boiling water can hold a bit more and then it will precipitate out with the Harmalas.
 
Eden
#58 Posted : 6/28/2010 9:31:37 PM

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This method worked best for me:
-Salt (first salting involves the slowest filtering)
-Redissolve and filter multiple times (filtering will get progressivley easier)
-Freebase (with most of the larger contams removed in the last step, filtering will be quite easy)

Repeat any steps any number of times as desired.

The excess salt can and will be carried over, but afaik the sodium carb precip will not pull out the excess NaCl in solution.
 
MelCat
#59 Posted : 6/16/2011 7:26:51 PM

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Just curious, is step 10 in the wiki kinda unnecessary?

Provided that the brew is properly filtered and reduced, could you just go strait to step 12 and do the salt precip?
Convert a melodic element into a rhythmic element...
 
endlessness
#60 Posted : 6/16/2011 8:52:15 PM

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You can, but.. If you start with salt precipitation, it can be hard to filter (sometimes it doesnt settle nicely to decant), so doing a first base precipitation will make the first filtering a bit easier, and once you do the salt precipitation it will be cleaner to filter. I used to go straight for the salt, because I had my filtering tricks (vacuum, being patient, more than one filter/funnel at once, moving the bottom sediments once in a while, keeping a large liquid volume on top of filter to speed filtering due to gravity, etc), but a few people like gibran have brought to the attention that doing a first base precip helps, specialy if its lye, so I added to the wiki. Feel free to do as you please Smile
 
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