Harmala solubility, acid/base

[Asher7]

Hello,

I was recently extracting some Rue seeds and noticed when I grow the crystals out after the Manske there is a darker “sludge” in the very bottom of the glass, but when I switch it over to FB there aren’t any dark spots. First thought is it’s just getting distributed throughout the FB but if you let the cup sit to settle before basing nothing settles. Second thought is they may be the very first crystals that formed mid water and fell, maybe making them look darker and without the fiberglass look? I’m really not sure and figured one of you guys would know.

 

[Jees]

Pictures say more than words
I'll throw my best bet:

Before the manske, is the acid liquid filtered finely?
* cotton ball in funnel neck;
* or poring it 5 x trough same coffee filter (gets finer each time).

If the liquid comes trough super clear, then you can't get much of a surprise during manske, then all you can get is good material (except for salt contamination).
I'm not saying it must be always that clear to do a manske, but in your case that could rule out doubts.

The final outcome how your harmalaHCL will look is a bit dependent on circumstances. Concentration of salt, of harmalas, of their purity, the temperature curve you followed, ....

 

[blue.magic]

This happens to me too.

One way to reduce this is to redissolve crude FB (not Mansked yet) in small amount of acidic water (vinegar) and re-filter it. It will capture more sludge and impurities.

Cotton balls and coffee filters won't remove the finest impurities. I actually filtered the tea many times and then passed the clear tea through a bed of Celite (vacuum filtration setup) - the Celite turned brown and captured a film of sludge that so far passed all filters.

The impurities will go away naturally with successive recrystallizations.

 

[Asher7]

This is well into the process so everything’s been filtered about as well as it’s going to get with what I have available, after when in the fb state is past the light brown/tan stage and at the white/slightly tan. That’s why I thought it may just be getting dispersed in the fb, but falls out of the acidic salt crystal form. Either that or it’s just the first midwater crystal fragments that fall to the bottom, because they dissolve immediately in vinegar and if you see the water before basing it there’s nothing in there.

 

[blue.magic]

That looks like pretty damn pure freebase :thumb_up:

if you see the water before basing it there’s nothing in there

Here is an image of my filtered tea, which passed the finest filter. Yet just adding salt pushed lots of impurities out of the solution (see the left beaker). You can also see the sludge settling on bottom, maybe similar to whay you described in OP.

This is why the actual purity can be granted only after several Manske crystallizations.

I wonder what these impurities are, but likely some partially water soluble stuff that cannot be completely washed out from freebase.

 

[Asher7]

That’s exactly what it looks like too, a grainy dark sludge. It’s possible to get out because it sinks but it’s going to cost you some final weight. I thought maybe I over did the salt the first time. I guess next time I have the chance I’ll separate it and see if you can base it.

Another possibility I’ve thought about is it being a separate alkaloid because there’s processes to separate the different alkaloids in there. I’m sure somebody here will know.:thumb_up:

 

[Jees]

... passed the clear tea through a bed of Celite (vacuum filtration setup) - the Celite turned brown and captured a film of sludge that so far passed all filters...

Thank you for mentioning the extra mile, love to learn geek :thumb_up:

 

[Asher7]

Looks like I may have found my answer.

Hello.
As far as manske, this is how I like to do it: once acidified simply add salt to get to ~20% NaCl or more. Fine crystals/powder should crash out quickly. Put the jar in a pot with water on the stove top and let the water in the pot get to a boil. Eventually the fine powder in the jar will redisolve thanks to the heat. Then turn off the heat and leave everything alone (e.g., overnight). After a few hours it will be at room temp, then move it to the fridge. The next day there will typically be long needledls thanks to the slow temperature drop and crystalization. Remember Jees mentioned the temperature profile in another post? A slow cool down from a saturated solution seems to work well.

I’m going to venture a guess that’s my culprit. I just salted some a minute ago I could try the reheat trick on but I don’t think I trust the glass’s ability to handle being double boiled, it’s just a normal drinking glass. I need to find a clear thick mug.

 

[Loveall]

I used a mason jar. To be clear you only need to heat up the liquid so everything redisolves, and that may happen even before the outside water boils but that was not my experience. You probably already know this, but heat everything together to avoid a shock (don't put a cold mason jar in hot boiling water).

 

[Asher7]

See it down there? I’m guessing this would be the point where I turn on the heat and remelt that powder. So it’s harmala hcl then and ok to just mix in with the dried crystals? Potency is equal mg for mg?

 

[Loveall]

I can't say what it is at this point. If it dissolves with heat and turns into long needles when allowed to slowly cool it's most likely Harmine/Harmalime HCl.

When adding salt to plant extracts proteins can crash out so there are other possibilities. Did you manske right away or did you base first?

 

[Asher7]

I based this one first. Is there an advantage to salting it first? I went ahead and grew these crystals out and strangely enough it looks like I didn’t get a dark spot. I think remembering back I may have pulled out the dark spot a few months back when making it. I’ll keep experimenting around and try reheating it once I get a glass I trust.

 

[Loveall]

Basing out first like you did is good, it makes it less likely that what you have after salting has proteins and other unwanted stuff.

There are other ways to heat up the water. Maybe consider a microwave? Good luck.

 

[Asher7]

I never thought about a microwave. A good heavy jar is probably something that will prove useful in the future, I have no idea what mason jars are rated for heatwise off the top of my head.

So I’ve had these hcl crystals drying for awhile now and can already see one thing I overlooked. I didn’t squeeze all the water out of the crystals/filter and a lot of the salt came over onto my tray. So my weights will be a little off. I did the whole thing food safe so I dipped my pinky into those clear crystals and sure enough salt. I’m not overly concerned except I think one of the things to avoid when taking harmalas is high amounts of salt. I may just regrow them.

So lesson learned, when finalizing hcl after a manske get all the water out.

 

[Jagube]

I’m not overly concerned except I think one of the things to avoid when taking harmalas is high amounts of salt.

This is not a safety concern at all, but a spiritual diet proscription. And it may be more for historical than any other reasons. The indigenous people didn't know salt until the European conquerors brought it with them. In the context of Ayahuasca drinking, which was associated with jungle life and the indigenous ways, things that came from the whites were seen as somehow 'impure'.

If your harmalas are even 50% contaminated with salt, you'd still only be consuming ~210mg of salt with your dose (assuming a dose equivalent to 180mg freebase), 5% of your daily RDA.

 

[Jees]

The colour is spot on :thumb_up:

You might dissolve again and freebase it to keep it as a freebase.

If you prefer HCL form: what you can do to minimize salt contam, put the yellow pile in a coffee filter and put paper towels under and above the coffee filter, add weight (books?).
Swap paper towels if they got wet. It sucks out much of the water + salt.

 

[Aum_Shanti]

It sucks out much of the water + salt.

Yep, I also always do it that way.

I also always do some rinsing with less salty water after filtering, to get less salt contamination. AFAIR you can also do a HCl acid rinse.

 

[Asher7]

Oh ok that’s good to hear, I was worried it may kick off a high blood pressure migraine or something similar which I imagine would be terrible amplified my harmalas etc. It looks like a good bit settled around the outside so I just tossed that and kept the solid chunk. I’ve yet to taste to get an idea of how salty but I diluted the plate leftovers in a shot of water and it wasn’t overly salty so I think you’re right when you say it’s not a problem causing amount.

I stored 90% as fb out of convenience and switched over 750mgs to hcl for an allergy test/oral ingestion. Is this similar to what I’ve read about other extracts where hcl stores better overtime? Fb compacts down much tighter which is nice. Chances are if it doesn’t go bad in 7-8 months it will be fine either hcl or fb I would think.

And the book idea is perfect, I noticed I could scoot it around and the “fibers” would hold it together so I’ll take your advice next batch and press it between some weights.:thumb_up:

I guess there’s no putting it off any longer, start with 50mg and see what happens? Then jump to 100 and then jump in 25mg increments? Sounds responsible.

 

[Jees]

...I guess there’s no putting it off any longer, start with 50mg and see what happens? Then jump to 100 and then jump in 25mg increments? Sounds responsible.

I find 50 mg noticeable good effects, kind of a soft headspace. With 100mg I can still do a job without problem but this is kind of the limit to be busy on, then I rather have free time to enjoy the headspace, not trippy though.

Happy trials!

 

[Asher7]

A little follow up.

So I did an allergy test, 150mg total in 50mg doses 30 minutes apart. Then a separate time 100mg at once, and finally 200mg total in 100mg doses 30 minutes apart. Very noticeable effects, similar to kratom where there is a sedation but also a lift of energy at first. Good for meditation I bet. Only on the high dose did I get any nausea but it was that preflight adrenaline purge type of nausea and not the flu kind so all was well. Afterwards a little bit of a headace/hangover but minor.

A few interesting tidbits, on the last two doses a bit of dmt was added simply to gauge if the harmalas were doing as intended so second to last was 15mg. Static in the air, visual changes etc, could be it, could be harmalas. Last dose 30mg was added, it was late and the harmalas were doing a real good job at sedation and I half drifted off to sleep. Real quickly my vision changed into a horizontal nature and opened real fast, as that happened over to my left a quick flash of a head leaned up to my ear and said what I have concluded was “Shooooo” and I startled awake. I could feel the puff of air in my ear like would happen if someone actually did this.

I have dreams that are way out there so something like this could just be my head doing it’s sleep thing but it made me chuckle that under the circumstances it would materialize like that.

So, my concern now is deciding whether the 30mg kicked in and was mild for me, so increase, or didn’t and keep at 30mg. I’d like to not waste but also dont want to finally get the inhibition right and overkill on the other going kaboom.

Edit - Something I just considered was back in the beginning a year and a half ago with my first attempt smoked I may have gotten a little disrespectful and over hit twice, causing me to get half way through the thought of oh s..blacking out. Maybe I’m still blacklisted in hyperspace. That would be sad.