Rue extraction fail

[klaupacius]

I am trying to extract harmalas from rue for the first time and I have run into a weird problem. I am following Sakkadelic's tek and have just finished the manske (12 hours) and dried the filter. Instead of an expected ~6g yield from 100g seeds, I have only 1g of red (not orange) colored crystals (they did look really nice in the jar). I think I followed all the instructions to the letter and it's taken me three days, so I'm really frustrated. What could have gone wrong? I did save the water layer from the manske jar, maybe more crystals are recoverable from there?

Alternatively, can anyone recommend a rue extraction tek that doesn't either require hours of painstaking filtering or four days of work?

 

[klaupacius]

Also, is it safe to freebase and use the red crystals, or are they too impure or something?

 

[Hyper Turtle]

Yeah let it sit another 24h and see what happens. Sometimes manske can be slow. You could also reduce it by maybe 30% before you continue the manske.

The red crystals will probably become nice beige to near white freebase.

For your next extraction, i can recommend NOT grinding or mashing the seeds, but simmering the whole seeds for an hour or more, in ample water that's slightly acidic, at least 3 times (i like to add 2L per 100g seeds and simmer until it's reduced to half, 3 times). Also i recommend, instead of super tedious filtering, just strain it through a cloth, squeeze the water out of the seeds without bursting too many, then let the strained liquid sit for 12h+. That will settle most of the sludge, and after that it usually passes through a coffee filter alright.

I don't know of a way to get harmalas quickly, but if you give everything extra time at each step, you can get them without much work. I like to do one simmer each evening, crude-base these (with lye) separately each after sitting until the next evening, then combine all the freebase for the Manske and final base (with ammonia).

 

[murklan]

I don't know of a way to get harmalas quickly, but if you give everything extra time at each step, you can get them without much work. I like to do one simmer each evening, crude-base these (with lye) separately each after sitting until the next evening, then combine all the freebase for the Manske and final base (with ammonia).

Sounds like a good arrangement! Will try that. Any specific reason to use ammonia?

 

[Hyper Turtle]

I have two reasons for using ammonia:
- i can smell if i didn't wash the freebase enough
- if there's any traces of it in the product, they'll evaporate

Not that there's anything wrong with using sodium carbonate or whatever, it just gives me extra peace of mind.

 

[murklan]

Yep, sounds like good reasons. I have it and will try in the next extractions. Thanks.

 

[klaupacius]

Yeah let it sit another 24h and see what happens. Sometimes manske can be slow. You could also reduce it by maybe 30% before you continue the manske.

The red crystals will probably become nice beige to near white freebase.

For your next extraction, i can recommend NOT grinding or mashing the seeds, but simmering the whole seeds for an hour or more, in ample water that's slightly acidic, at least 3 times (i like to add 2L per 100g seeds and simmer until it's reduced to half, 3 times). Also i recommend, instead of super tedious filtering, just strain it through a cloth, squeeze the water out of the seeds without bursting too many, then let the strained liquid sit for 12h+. That will settle most of the sludge, and after that it usually passes through a coffee filter alright.

I don't know of a way to get harmalas quickly, but if you give everything extra time at each step, you can get them without much work. I like to do one simmer each evening, crude-base these (with lye) separately each after sitting until the next evening, then combine all the freebase for the Manske and final base (with ammonia).

So the tek is:

1. Simmer 100g whole seeds in 2L acidic water (is 1 tbsp white vinegar enough?) until reduced to half
2. Strain and squeeze seeds gently
3. Wait 12-24H for sludge to settle, decant liquid leaving sludge behind
4. Add lye until solution turns milky
5. (Here's one I'm confused about--do you wait for precip or filter immediately?)
6. Repeat steps 1-5 2+ times
7. Combine precips from step 5
8. Manske
9. Filter and dissolve crystals in acidic water
10. Add ammonia until solution turns milky
11. Wait for precip, filter, dry thoroughly, use

Is that right?

 

[klaupacius]

Also, do I need to do the water washes from Sakkadelic's dek after step 7 and 11? And can I just run those through a coffee filter right away or do I need to wait more time to settle?

 

[downwardsfromzero]

I'd say for step 3 you'd decant into a filter. Also, you appear to have steps 8 and 9 the wrong way round. The combined precips get dissolved in acidic water, then you add brine for the Manske (best if the alk solution is around pH 4 at that point).

It can help to do water washes on the precipitated base, although I've found this loses a significant amount of the finer precipitate.

Settling and decanting, or even better, syphoning is a viable alternative to filtering, especially if filtering turns out to be tediously slow - which with harmalas often turns out to be the case. somehow rue produces ongoing amounts of fine, sticky, powdery crud that seems designed to clog filters. Btw, when I do filter - which is usually as an adjunct to dissolving freebase back into acidic solution - I tend to use a large polyethylene funnel with a cotton wool plug that is neither too tight nor too loose.