Freebase precipitation fail :)

[amazingino]

Hello all

I was trying to extract the syrian rue alkaloids and just totally failed the first precipitation stage.

I don't really know what went wrong, so if someone can try to spot the error, it will be great.

1) I freezed 25g Syrian Rue seeds for 24h and ground them into fine powder.
2) Boiled in fresh tap water for 2h, decanted and boiled 2h again with more fresh water.
3) Water of both batches thoroughly filtered through multiple cottons/coffee filters and all solid mater discarded, I obtained 300mL of dark yellow rue water.
4) sodium carbonate solution was made by first transforming NaHCO3 to Na2CO3 (I cooked it at 100°C in the oven for 1 hour) and then saturating 200mL of water with it then filtering through coffee filter in order to remove excess sodium carbonate.
5) Adding very slowly the sodium carbonate solution to the rue water produced no precipitation at all, I finally poured the total of 200mL of it with no signs of precipitation.

I have obviously done something wrong, maybe the NaHCO3 to Na2CO3 transformation was not complete, but even NaHCO3 solution should produce at least a bit of precipitation right?

What you think about it?

 

[endlessness]

Here's a few possibilities, it could be any of them or a mix:

- Bunk seeds (reputable supplier or anybody tried before from batch?)

- Your tap water too basic, so alkaloids are less soluble in it (add acid like vinegar last time)

- 2 boils are not enough, do 3 or 4.

- Conversion of bicarb wasnt enough, next time weigh before and after, and maybe try 200c instead of 100.

Was there any change of color as you added the base solution?

Do you have anything to measure pH?

Do you have some lye at hand?

 

[amazingino]

Here's a few possibilities, it could be any of them or a mix:

- Bunk seeds (reputable supplier or anybody tried before from batch?)

This is a possibility, ATM I am ordering 2Kg from no suppliers - thanks, MOD

- Your tap water too basic, so alkaloids are less soluble in it (add acid like vinegar last time)

I forgot to say, but I added some lemon juice in order to acidify the brew a bit, I don't think this was the problem.

- 2 boils are not enough, do 3 or 4.

I'll do that next time, but I'm pretty sure most of alkaloids should be pulled by two boils.

- Conversion of bicarb wasnt enough, next time weigh before and after, and maybe try 200c instead of 100.

This is probably the fail step indeed. I was pretty sure that bicarbonate should work, but tried the conversion just to be sure. I am also ordering the "real" sodium carbonate for next try.

Was there any change of color as you added the base solution?

Do you have anything to measure pH?

Do you have some lye at hand?

No change in color, no pH meter (I just ordered one out of frustration ) and no lye. Is lye really necessary? I would like to avoid non food-grade ingredients if possible.

Thank you for your help, I'll wait few days and retry with new pH mater, new seeds and real sodium carbonate.

 

[endlessness]

Maybe what happened is you added too much lemon and that the sodium carb (or worse, bicarb) was not enough to neutralize the acid and then basify. Make more sodium carb, and add it to the brew, see if some precipitates.

Lye was just one possibility because you would only need a little, and it would easily get the pH high enough, so if alks are there, they would precipitate.

An advantage of lye is that it precipitates cleaner crystals than sodium carb.. For me, the best way to extract rue is alternating base and salt precipitation a couple of times, and the first time or two, use lye as a base, and then the last one use sodium carb because thats 'safer' to consume (even though just washing the freebase harmalas with a dilute sodium carb solution should get rid of any lye remains)

let us know how it goes

 

[amazingino]

I've made more sodium carb solution (600mL) and slowly added it to the mix. No immediate precipitation but there was some solid matter at the bottom layer the next day. I tried to dissolve it in FASW with partial success and finally discarded everything as it was getting out of control

I just bought some lye (NaOH), I will try that as soon as I get new seeds.

Thank you for your help friend

 

[PrimalWisdom]

I'm no rue extraction expert, but I had difficulty precipitating enough alks with sodium carbonate - I used Lye and voila - a hell of a lot of alks precipitated out.
I just cleaned up my harmalas with water a few times after I was done and my harmalas are awesome - for cleaning up harmalas check out the caapi extraction thread - somewhere on the site :/

 

[amazingino]

Meanwhile, I've extracted harmalas from cielo caapi liquid extract 5:1 using gibran2 tek. First pull with lye, and second with sodium carbonate and wash until 8 pH (I also have the pH meter now so it is a lot easier).

With sc it was a lot slower, but at least it is safer.

I just came from a journey with 15mg vaporized harmalas 30mn prior to 7mg vaporized DMT. Very profound and lasted very long time, something like 1h heavy mental/visual effects after 5-10mn near breakthrough experience in presence of multidimensional geometric entities. I meditated a lot and learned a lot from this experience. At some point I re vaporized more DMT with another near break through. It seems that vaporized harmalas last very long time, 2 hours maybe more.
I think I found my magic combo

I'm still waiting for Syrian Rue in order to retry with lye/sc combo.