Hello nexus community,

This is my first post and my first real extraction.
I'm using 500g of finely powdered bark which I more or less cooled in the freezer took out and let thaw like 2 times.
Unfortunately I did not realize that the freezer was maybe a little too warm, but whatever.
The main reason why I'm writing this is to mention that theoretically I thought everything will be kinda not too hard but as almost always practically its a much more different thing. So that should be actually no surprise.
Acidifying with phosphoric acid got fine, except that the solution got maybe a liitle too acidic, like between 2,3 and 2,9.
I boiled 3 times for ca. 2h and reduced the amount of solution to ca. Half a liter. So far so good, then I realized that I only had calcium hydroxide and NaCO3. So I tried with NaCO3 but I had to add a very high amount of that plus water to the half a liter acidic solution and finally ended up with a ph not wanting to get above 10,6 or so, BUT the solution got black, actually really black.I read that black color is a good indicator, but that low ph makes me unsatisfied. Surprisingly if found a little NAOH but only a very small amount, nevertheless I added it but the max ph I could get was about 11,6, maybe 11,7. And I had about 5 liters now to deal with, which only found space in 3 separat buckets, That are 2 lab grade glasses and one crockpot out of stainless steal (hope that's ok with the basicity of the solution???). Ah and I have to add that before I added the NAOH to the solution I tried to add some Calcium hydroxide, which I know should only be used in a dry tek, but it was not much, but whatever, after a while I checked whether there a clumps of something that have not been gotten dissolved, at the bottom of the buckets. And there was.
How can I deal with those?
My plan now is too pull with limonene and get the alks that are already there and later maybe acidify all the 5 liters in the buckets, reduce them to a workable-with amount of solution and hoping that the clumps have gotten dissolved again somehow maybe, I don't know whether that would work. Then basify with NaOH to get a ph of maybe 13 and pull the rest of the alkaloids if there are any then.
I also only have a 1 liter separatory funnel, so I would use 500 ml of basified solution and pull with limonene. But as I have 3 buckets with like ca. 2 liters in one bucket, I think of doing actually 4 pulls with 40 ml limo each for the first round.With Each pull swirling ca. 1h. Then a second round and a third would follow with each round lasting for 24 hours.And all this I would do with the other two buckets as well. That would be 480 ml limo-pulls but only for 2 liters. I have five. So how should the quantity of solution together with the ability of the separatory funnel influence the decision of the number of pulls to be taken and the quantity of none polar solvent to be used for each single pull? I know I would not think about this that much if I had less liters to be dealing.

Thanks for any suggestions and I wish all the best to all in this forum and hopefully very successful future experiences.

Dont worry about the undissolved calcium hydroxide, maybe some of it reacted with sodium carbonate to form even more lye, which is good because it would further raise the pH. At 11.6, you're gonna get some alkaloids but possibly a significant amount not. Or it might have more chances of emulsion. You can try doing the pulls and then later adding more lye and doing more pulls. I wouldnt acidify/reduce/basify again because it seems like youll be using a lot of acid to neutralize the bases, and then base again to neutralize the acid. If you just raise the pH and do thorough cycles of mixing in each pull, you should have a good yield.

When extracting, always have a few extra glass jars standing around if you deal with unexpected amount of liquids or if you have to dissolve substances.

If your separatory funnel is not big enough, just do the separation in two rounds, or get a bigger one next time. The size of pulls, for 500g mimosa, I would do 100-200ml pulls, and do at least 4 or 5, and then do yet another one but salt from it separately to see if there's still a significant amount of alkaloids in the last. If so, do a couple more long pulls, till no more alks come out. But of course this probably means having the basified mix for at least a few days there as you work on your extraction.

How are you planning to salt your alkaloids out of the limonene? I would suggest checking BLAB tek if you didnt.

Thanks for the Tips, endlessness.
Yes, acidifying again , reducing and basing again would indeed mean to deal with a lot of stuff again, so I will follow your advise and just basify more right away when I have hands on NaOH. Soon I will have the opportunity to work with a 6 liters boiling flask, so I will be able to work with a lot in a single container.
Concerning your question how I will salt the alks out of the limo, i will salt with Fumaric acid after which I will let the alks precipitate right out of water in the fridge, as described in the BLAB TEK.

After what time of letting a basified mix stand around do you think it becomes a problem like leading to a loss of alks?
And considering making 5 pulls like you suggested, do you think it is ok to do the 3 first pulls within approximately 3 hours and the last two throughout 2 days?
I am experiencing the layers separating very fast, already after 10 mins. So the separating/mixing process would occur many times already during one hour.