Freebase harmalas not setttling

[Northerner]

I don't know why but the last couple of times my freebase alkaloids won't settle properly. The alkaloids become so fine that they remain suspended and can take weeks to settle. In fact the last extraction I just put in the cupboard and forgot about because I was sick of watching it.

What could be the issue? Did I not filter enough before basing? How to fix it?

This has never been an issue before this year.

These pics are 12 hours after decanting. I put 2 decanted jars showing about the same amount of settled harmalas into a jar with fresh water. Now half of it is suspended. Looking in the top you can actually see it floating around in there.

 

[Eaglepath]

Sometime ago I did this now but cant you just pour it through a coffe filter and it will collect the material?

 

[pastanostra]

Did you try fridge for a day or two ?
It's generally what i've done and inthink it helped a bit. Of course i've sawn alks floating but not so much.

 

[monomind]

I did only one 2 harmala extractions in my life so far, so take my answer with a huge grain of salt, but in your first pic the aqueous layer looks like it is full of gunk. Why do you think it is alks floating there ?
If I was in your situation I would acidify the liquid to dissolve the alks, filter everything through a coffee filter, manske it ( if you are working with rue ) and then base again.
BTW, What raw material you used ?

 

[Northerner]

Already I had figured and done what you said monomind

I knew there was alks in there because I had decanted and combined 2 jars that were showing the same amount of settled alks you can see in that pic. It was hard to capture on a camera but I could see the alks swirling in the aqueous layer if I gave it a tiny stir.

I decanted the liquid and filtered it, recovered a pile of not so flash looking harmala. Melted the whole lot down, filtered a few times and mansked it. Is in deep cool in the fridge now.

It seems the quality of seed I get these days isn't like it used to be. Much more crap and much less harmala. From 500g I'd easily get 20-25g of harmala before but I'm lucky to get much more than 10 these days.

There's a range of things going on.

 

[Northerner]

So, if you guys want a bit of a laugh...

I filtered out the xtals from the manske and was looking at the aqueous solution. I could try and manske it again to recover any remaining alks I thought, but why not just base it and precip them if they exist they'll come out right? Lol. I know one doesn't mix acids and bases, but was a bit of a momentary lapse of reason.

So I dump a heaped tablespoon full of sodium carbonate in a large jar vinegar and gave it a nice big stir. :lol:

Oooh, I thought. Look how much is there it's turning so white... Oh my, it's rising. Oh fuck get it to the sink quick! The jar more than half emptied itself in the sink in seconds. Just a few inches of solution left after the bubbles subsided. A moment later that would have been on my kitchen bench.

 

[Northerner]

Fixed it. Was more drama and less yield than usual though.

 

[Eaglepath]

Wow.. that's a big pile8)