BongQuixote
Rising Star
Happy New Year!
Here are some notes regarding VDS protocol. I've done it 5 times so far, and I could use help peer-reviewing some of my findings.
Boil: I do 5 one hour boils with 7% vinegar. I found that the amount of vinegar suggested by VDS was barely enough to saturate the seeds during the first boil, so got almost no liquid left. I advise doubling the amount of liquid across all the boils. With more diluted liquid trapped in the seeds, less loss of product. I also sparge the grains with hot water after the final boil to rinse out any harmala containing liquid in the seed mass (learned that from brewing beer). I do all my boils in a pressure cooker with the lid closed, but not locked, during boil 1-3 and with the lid locked and 15 psi pressure during boils 4-5. I started doing this with Acacia bark and my yield jumped 30%, so I kept that practice with rue seeds. Having the lid on also prevents the entire house from smelling of vinegar. I also don't grind my seeds. Looking at the VDS results, it doesn't seem to increase the yield enough to be worth the extra mess.
Reducing: I reduce down to one liter for 500g of seeds.
Filtering: First through t-shirt fabric multiple times, then through coffee filters and finally through medium filter paper using a Buchner funnel and vacuum. I save all the filter material and squeeze out any liquid from it. Then I rinse the filters in vinegar and combine that with the squeezed out liquid, let it sit overnight to let sediment settle and then decant off the supernatant and run that through the medium filter paper. Combine that liquid with the filtrate and filter one more time for good measure. This takes me about 2 days, since the first two filtering steps are gravity powered. Just let it sit and drip overnight. I go through maybe 3 t-shirt pieces and 3 coffee filters to get everything through.
Initial basification: I use lye added under magnetic stirring, being careful not to get the liquid too hot. I stop when I get to PH 10 and let cool. I use the same PH meter as VDS, great piece of equipment for the money.
Manske: I follow VDS here regarding method and amounts, insulating the jar while it's crystallizing and sticking it in the fridge after it has reached room temperature (after 8-10 hours). After each re-dissolving I filter the liquid and squeeze out any remaining liquid from the filter. I also save the salty water from the previous round, reduce it down 30%, add some more salt, and give it another round of crystallizing. So I effectively do a double-check to make sure everything mansked out right. Only once did I find any extra crystals during the "verification manske", but it's a easy step and it doesn't delay the process. I manske five times. The previously mentioned red goop usually shows up at the bottom after manske 2 or 3, and it doesn't redissolve so easy to filter out. It tends to have crystals stuck to it, so I don't want to leave it at the bottom of the jar.
Harmine/Harmaline separation: I add 12% ammonia dropwise under magnetic stirring, going slow. It takes me maybe 15 minutes to complete it, with no more that one drop per second of ammonia being added. I found that adding ammonia too fast causes harmaline to precipitate out early, due to locally higher PH in parts of the solution. This become especially important as you get closer to your precipitation point and the PH of your solution is no longer acidic enough to redissolve any accidentally precipitated harmaline. Go slow, it pays off.
Adding ammonia dropwise, keep an eye on your PH meter. Make sure each addition of ammonia causes a rise in PH. You need to give the ammonia time to distribute throughout the solution and for the PH meter so stabilize, so don't go too fast. You will eventually see a PH drop and clouding of the solution. PH might drop pretty far, almost a full point isn't uncommon. Give the solution some time to stabilize and keep adding ammonia dropwise. After each ammonia drop, make sure the PH returns to the same exact value it had before you added the drop. If the PH stabilizes at a higher point, keep adding ammonia until you're around 0.2PH higher than the stable point you identified earlier. This may only take a 1-3 drops. Most harmine should now be out of solution. I've seen this happen as low as PH 5 and as high as 7.
Filter and save your harmine. Add more ammonia dropwise, still being gentle, until you get to PH 9.8 and then filter out your harmaline. This got me a 54/46 ratio between harmine and harmaline, which seems top be consistent with most people's results. I rather stop the harmine precipitation a little earlier than risk getting harmaline in my harmine. Having some harmine in the harmaline is less of an issue for me.
Starting with 500g of seeds, I got 7 grams harmine and 6g harmaline, so a 2.6% yield. Product is very clean with no pigmentation, oils or plant matter left.
After doing this I went back to my old "mixed harmalas" jar and reprocessed everything from the manske steps onward. I lost over 30% of my product, but that was due to the fact that my previous process was sloppy, only 2 manskes etc, so it removed mostly impurities. The I converted half the harmline to THH per my previous post. I find that doing the magnesium reduction to THH works best when you start with clean harmaline.
I did do the sodium carbonate and sodium bicarbonate methods as well, but it was just way too messy for my taste. I think those are great for safety reason, and I will recommend them to any one doing this for the first time since it's hard to hurt yourself by doing it wrong.
Thanks for the note, Elrik. I will try your experiment!
Here are some notes regarding VDS protocol. I've done it 5 times so far, and I could use help peer-reviewing some of my findings.
Boil: I do 5 one hour boils with 7% vinegar. I found that the amount of vinegar suggested by VDS was barely enough to saturate the seeds during the first boil, so got almost no liquid left. I advise doubling the amount of liquid across all the boils. With more diluted liquid trapped in the seeds, less loss of product. I also sparge the grains with hot water after the final boil to rinse out any harmala containing liquid in the seed mass (learned that from brewing beer). I do all my boils in a pressure cooker with the lid closed, but not locked, during boil 1-3 and with the lid locked and 15 psi pressure during boils 4-5. I started doing this with Acacia bark and my yield jumped 30%, so I kept that practice with rue seeds. Having the lid on also prevents the entire house from smelling of vinegar. I also don't grind my seeds. Looking at the VDS results, it doesn't seem to increase the yield enough to be worth the extra mess.
Reducing: I reduce down to one liter for 500g of seeds.
Filtering: First through t-shirt fabric multiple times, then through coffee filters and finally through medium filter paper using a Buchner funnel and vacuum. I save all the filter material and squeeze out any liquid from it. Then I rinse the filters in vinegar and combine that with the squeezed out liquid, let it sit overnight to let sediment settle and then decant off the supernatant and run that through the medium filter paper. Combine that liquid with the filtrate and filter one more time for good measure. This takes me about 2 days, since the first two filtering steps are gravity powered. Just let it sit and drip overnight. I go through maybe 3 t-shirt pieces and 3 coffee filters to get everything through.
Initial basification: I use lye added under magnetic stirring, being careful not to get the liquid too hot. I stop when I get to PH 10 and let cool. I use the same PH meter as VDS, great piece of equipment for the money.
Manske: I follow VDS here regarding method and amounts, insulating the jar while it's crystallizing and sticking it in the fridge after it has reached room temperature (after 8-10 hours). After each re-dissolving I filter the liquid and squeeze out any remaining liquid from the filter. I also save the salty water from the previous round, reduce it down 30%, add some more salt, and give it another round of crystallizing. So I effectively do a double-check to make sure everything mansked out right. Only once did I find any extra crystals during the "verification manske", but it's a easy step and it doesn't delay the process. I manske five times. The previously mentioned red goop usually shows up at the bottom after manske 2 or 3, and it doesn't redissolve so easy to filter out. It tends to have crystals stuck to it, so I don't want to leave it at the bottom of the jar.
Harmine/Harmaline separation: I add 12% ammonia dropwise under magnetic stirring, going slow. It takes me maybe 15 minutes to complete it, with no more that one drop per second of ammonia being added. I found that adding ammonia too fast causes harmaline to precipitate out early, due to locally higher PH in parts of the solution. This become especially important as you get closer to your precipitation point and the PH of your solution is no longer acidic enough to redissolve any accidentally precipitated harmaline. Go slow, it pays off.
Adding ammonia dropwise, keep an eye on your PH meter. Make sure each addition of ammonia causes a rise in PH. You need to give the ammonia time to distribute throughout the solution and for the PH meter so stabilize, so don't go too fast. You will eventually see a PH drop and clouding of the solution. PH might drop pretty far, almost a full point isn't uncommon. Give the solution some time to stabilize and keep adding ammonia dropwise. After each ammonia drop, make sure the PH returns to the same exact value it had before you added the drop. If the PH stabilizes at a higher point, keep adding ammonia until you're around 0.2PH higher than the stable point you identified earlier. This may only take a 1-3 drops. Most harmine should now be out of solution. I've seen this happen as low as PH 5 and as high as 7.
Filter and save your harmine. Add more ammonia dropwise, still being gentle, until you get to PH 9.8 and then filter out your harmaline. This got me a 54/46 ratio between harmine and harmaline, which seems top be consistent with most people's results. I rather stop the harmine precipitation a little earlier than risk getting harmaline in my harmine. Having some harmine in the harmaline is less of an issue for me.
Starting with 500g of seeds, I got 7 grams harmine and 6g harmaline, so a 2.6% yield. Product is very clean with no pigmentation, oils or plant matter left.
After doing this I went back to my old "mixed harmalas" jar and reprocessed everything from the manske steps onward. I lost over 30% of my product, but that was due to the fact that my previous process was sloppy, only 2 manskes etc, so it removed mostly impurities. The I converted half the harmline to THH per my previous post. I find that doing the magnesium reduction to THH works best when you start with clean harmaline.
I did do the sodium carbonate and sodium bicarbonate methods as well, but it was just way too messy for my taste. I think those are great for safety reason, and I will recommend them to any one doing this for the first time since it's hard to hurt yourself by doing it wrong.
Thanks for the note, Elrik. I will try your experiment!
...I have the alkaloid mix for quite a while and haven't even tried it, because of the diet one should do...but 1 day is sufficient I guess of sparing out tyramine? Wanted to just use it subliminally as MAOI for the DMT experience.
