• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Failed Syrian Rue extraction

Migrated topic.
Dogbark

Dogbark

Rising Star
Hallo nexus ! Ive tried to produce an extract of syrian rue with the help of The Tao of Rue Extraction - DMT-Nexus Wiki. My only problem is that its impossible for me to aquire lye at the moment and i cant make any right now either.

So what i used in step 5 as a base were sodium carbonate and calcium hydroxide. I have approx 3 - 4 liters of liquid left.

First i added around 100g of sodium carbonate but i didnt see any color change so i added more in 10g increments up to 300g in total but again no color change. At this point i got impatient (huge mistake) and added 3 teaspoons of calcium hyroxide.

Is there any way to complete the extraction at this point ? Would be kind of a waste to throw away 1.6 kg of seeds.
 
Sort by date Sort by votes
Dogbark said:
Hallo nexus ! Ive tried to produce an extract of syrian rue with the help of The Tao of Rue Extraction - DMT-Nexus Wiki. My only problem is that its impossible for me to aquire lye at the moment and i cant make any right now either.

So what i used in step 5 as a base were sodium carbonate and calcium hydroxide. I have approx 3 - 4 liters of liquid left.

First i added around 100g of sodium carbonate but i didnt see any color change so i added more in 10g increments up to 300g in total but again no color change. At this point i got impatient (huge mistake) and added 3 teaspoons of calcium hyroxide.

Is there any way to complete the extraction at this point ? Would be kind of a waste to throw away 1.6 kg of seeds.
Click to expand...

Why did you start with 1.6kg of seeds? That's an insane amount of Harmala's? Last 200g extraction I did ended up with near 20 grams?
 
Upvote 0 Downvote
If you keep stirring, the Ca(OH)2 will eventually react. It just takes more time because it dissolves only a little at a time.

You may also want to add a lot more Na2CO3. The stuff you buy in the supermarket is usually the decahydrate, which in effect is more than 60% water. Keep adding the Na2CO3 (and stirring) until you do see the color change and precipitate forming. Let it settle, decant the liquid and filter the solids.

Don't worry about any excess Ca(OH)2 or Na2CO3 getting in the filtered precipitate. You should do another cleanup step anyway.

Dissolve the precipitate in a minimal amount of hot vinegar. Do this in small amounts, because any excess Na2CO3 in the solids will cause wild foaming when contacting the vinegar. Stir well and when adding more vinegar does not cause more solids to dissolve, filter the solution a few times.

You will now hopefully have a much smaller volume of liquid and you can either redo the base precipitation, or even better, do a Manske salting to get rid of the non-harmala alkaloids.

Tryptallmine: 20 gram yield from 200 gram seeds is a 10% yield and that sounds not realistic, from my own experience and from other postings on the forum. It probably contains a lot of impurities. 6% yield is very good, 4% is not bad for starters.
 
Upvote 0 Downvote
Dogbark,

I see now that I made a mistake. When Ca(OH)2 is added to Na2CO3, they react and form CaCO3. I expect that this is not going to react anymore at any rate with the dissolved harmalas, so it will be mixed in with any freebase that also precipitated.

I see two slightly different ways to salvage the mess:

- You could either add vinegar until everything, including the CaCO3 has reacted and redissolved as soluble acetate salt. Don't add too much acid at once, because as a result of the reaction, there will be lots of foaming from the CO[size=223[/size] produced. You can use some heat to speed up the reaction.

- Or you could add lots of base, until all of the freebase harmala has also precipitated. Then decant and filter the solids and dissolve them in acetic acid. Here too - watch out for the foaming.

Then do as the rest of the tek goes: add 100 gram NaCl for every liter of liquid and boil and stir until all has dissolved. Upon cooling slowly, harmala HCl crystals should form. The other salts will remain in solution. Cool slowly and let it stand for a day. Then filter the crystals.

The filtered harmala HCl crystals can be dissolved easily in hot water. Finally add the right amount of the right base. You should have harmala freebase sans the chalk.

It might make sense to do some added filtering after every dissolution step described above, you will have a nicer result further down the road if you do.
 
Upvote 0 Downvote
Two additions to the above post:

Perhaps a combination of the two methods that I suggested is even better: Decant and filter what has already been precipitated, and also keep the liquids. Then dissolve the filtered solids in acid and add the resulting solution to the remainder of original decanted/filtered liquid and do a Manske salting with the combined liquids.

The other addition is that the cross-elimination of Ca(OH)2 and Na2CO3 forms not only CaCO3, but also NaOH. The former precipitates, the latter remains in solution. This way, by carefully adding tiny bits of Ca(OH)2 at a time to a solution of Na2CO3 with good stirring, you can make a solution of NaOH (probably containing sizeable amounts of Na2CO3 as well).
 
Upvote 0 Downvote
Back
Top Bottom