Here I've combined elements from very conveniently simplified approaches by Sakkadelic and Brennendes Wasser into one method. I've reworked a couple of details, removed some unnecessary steps and added quick and easy salt and optional separation stages. In my opinion this is an easy, quick way to separated Harmine and Harmaline freebase of reasonable purity and good yields without grinding of seeds or filtering and reducing of large volumes of water. No funnels, no cotton balls and no extra back and forth between acids and bases.
Materials:
100G of dry Syrian rue seeds
Distilled vinegar, citric acid or fumaric acid or weak (<10%) HCl
Sodium hydroxide (lye)
Non-iodized salt (e.g. sea salt)
Sodium bicarbonate (optional, for separation step)
Sodium carbonate
Coffee filters
2X 1L mason jars or pickle jars and one extra jar (for filters full of harmalas to sit in and rinse).
A square of cloth such as a piece of an old T-shirt
pH strips or meter (optional but handy)
Turkey baster (optional)
Large saucepan
Water
-100g whole rue seeds in pan with about 1.2L of water.
-Add acid until pH3. If vinegar is too weak, you may use citric acid. I used <10% HCl. Without testing pH you can simply add a lot of acid (if it's not too strong), but pH strips are cheap.
-Boil for 3 hours and reduce to just about cover the seeds and decant into large mason jar through a piece of clean T-shirt cloth to trap larger particles.
-5 more 5 minute boils with only enough water to cover seeds. Adjusted pH with acid each time as needed.
-All boils should fit into 2 large mason jars (2/3rds full, leaving some room for lye solution).
-No reducing, no filtering. Base with lye solution. Clouding will form rapidly as the the harmala freebases, turning the solution milky.
-Alkaloids settle over a few hours. Add a small amount more lye solution. Stop if no more clouding occurs.
-Pour/ pipette (turkey baster) away as much water as you can without disturbing the settled freebase.
-Add fresh tap water and harmalas will settle again. Settling is faster each time. Repeat until the PH of the water is neutral. The color will be very faint.
-Collect and dry harmalas in coffee filter.
My yield was 7g of tan powder. Usually the yield would be about 5g with a lot of filtering in a normal extraction. From this current batch of seeds half of that would also be insoluble material which will be removed in the next step.
Manske:
-Dissolve freebase in 1 part distilled vinegar (roughly 75ml) in a pan on low heat, top up with 3 parts tap or distilled water (roughly 225ml).
-Filter solution through a coffee filter to catch dark insoluble material. From these seeds the insoluble material accounts for almost half of the crude freebase.
-Add filtered clear amber solution back into the pan and saturate with salt, stirring each spoonful until no more will dissolve at low heat (hot tea temp, below boiling).
-Pour solution into jar, leaving excess salt in pan. Rinse pan with tap water, fill and heat it. Sit the harmala jar this heat bath to slowly cool overnight.
-Next day, filter the crystals of Harmala Hcl and dry in the filter to obtain fine golden harmala HCl crystals.*
*Sakkadelic's drying tip: press the folded filter paper between paper towels to wick away excess water and salt. This is is useful if your desired product is the Harmala HCl as it is.
Separation of harmine and harmaline Freebase:
If you don't want to separate the freebases, simply skip ahead to adding sodium carbonate. This will force both alkaloids to crash out.
-Add crystals to pan and 200ml of tap or distilled water (pour through the filter which the crystals were recovered from to dissolve those stuck to the paper).
-Gently heat until everything is dissolved and filter into a jar through a coffee filter.
-Add 100ml of sodium bicarbonate solution (saturated at room temperature).
-Solution becomes slightly cloudy. Harmine begins to precipitate. More base solution can be added until no more precipitation is seen (it may take about 300ml total).
-Let solution settle for several hours then pour through coffee filter to collect harmine freebase.
-Rinse harmine 3x in the filter with cold tap water (as distilled water can be slightly acidic) to remove traces of sodium bicarbonate, then dry.
-Add sodium carbonate solution (saturated at room temperature) to the bicarb based tea. Pale harmaline freebase will crash out. Add more as needed (it may take 150ml this time).
-Let solution settle for several hours then pour through coffee filter to collect harmaline freebase.
-Rinse 3x in the filter with cold tap water then dry.
My yields: Harmine freebase: 1.9g. Harmaline freebase: 1.5g. Total 3.4% final yield after cleaning. Yield varies depending upon quality of seeds.
Notes:
I think a manske step is a good idea, and only one is necessary if everything was done correctly. Brennendes Wasser has shown some evidence that the insoluble remainder after adding acid is in fact just harmalas which won't dissolve for some unknown reason : Harmala extraction - unneccessary steps? . If this is the case, the dark insolubles could still reduce the effectiveness of a dose. In my opinion it does make sense to remove them. Further purification can be done to remove color, but if the product as pure as the tests have shown then it's more about cosmetics and will have little to no effect on dosage. That said, you can manske and base to your heart's content. For simplicity I haven't included such steps here. See The Tao of Rue Extraction or Harmalas Extraction and Separation Guide for info about this.
If you want to grow nice crystals but don't want to go back and forth with manske and base steps, you can do it as part of this method as a freebase. Simply add your base solutions very slowly over a much longer period of time and you will see small crystal clusters develop on the sides of the jar and on the surface of the solution. This is easy for harmine as the pH does not increase too rapidly with sodium bicarbonate.
I don't recommend adding sodium bicarbonate powder or oversaturated warm bicarbonate solution to a cooler harmala solution, as I have seen this cause excess sodium bicarbonate to flocculate as spongey masses that seem to trap dissolved particles, apparently including harmaline. Doing this after all the harmine had been exhausted, I noticed a color change from pale orange to a lighter yellow. Adding sodium carbonate after filtering the bicarbonate globs away did not precipitate anything as it should have. After redissolving the mass in another jar of water and adding sodium carbonate, harmaline did immediately precipitate.
Materials:
100G of dry Syrian rue seeds
Distilled vinegar, citric acid or fumaric acid or weak (<10%) HCl
Sodium hydroxide (lye)
Non-iodized salt (e.g. sea salt)
Sodium bicarbonate (optional, for separation step)
Sodium carbonate
Coffee filters
2X 1L mason jars or pickle jars and one extra jar (for filters full of harmalas to sit in and rinse).
A square of cloth such as a piece of an old T-shirt
pH strips or meter (optional but handy)
Turkey baster (optional)
Large saucepan
Water
Crude freebase extraction: -100g whole rue seeds in pan with about 1.2L of water.
-Add acid until pH3. If vinegar is too weak, you may use citric acid. I used <10% HCl. Without testing pH you can simply add a lot of acid (if it's not too strong), but pH strips are cheap.
-Boil for 3 hours and reduce to just about cover the seeds and decant into large mason jar through a piece of clean T-shirt cloth to trap larger particles.
-5 more 5 minute boils with only enough water to cover seeds. Adjusted pH with acid each time as needed.
-All boils should fit into 2 large mason jars (2/3rds full, leaving some room for lye solution).
-No reducing, no filtering. Base with lye solution. Clouding will form rapidly as the the harmala freebases, turning the solution milky.
-Alkaloids settle over a few hours. Add a small amount more lye solution. Stop if no more clouding occurs.
-Pour/ pipette (turkey baster) away as much water as you can without disturbing the settled freebase.
-Add fresh tap water and harmalas will settle again. Settling is faster each time. Repeat until the PH of the water is neutral. The color will be very faint.
-Collect and dry harmalas in coffee filter.
My yield was 7g of tan powder. Usually the yield would be about 5g with a lot of filtering in a normal extraction. From this current batch of seeds half of that would also be insoluble material which will be removed in the next step.
Manske:
-Dissolve freebase in 1 part distilled vinegar (roughly 75ml) in a pan on low heat, top up with 3 parts tap or distilled water (roughly 225ml).
-Filter solution through a coffee filter to catch dark insoluble material. From these seeds the insoluble material accounts for almost half of the crude freebase.
-Add filtered clear amber solution back into the pan and saturate with salt, stirring each spoonful until no more will dissolve at low heat (hot tea temp, below boiling).
-Pour solution into jar, leaving excess salt in pan. Rinse pan with tap water, fill and heat it. Sit the harmala jar this heat bath to slowly cool overnight.
-Next day, filter the crystals of Harmala Hcl and dry in the filter to obtain fine golden harmala HCl crystals.*
*Sakkadelic's drying tip: press the folded filter paper between paper towels to wick away excess water and salt. This is is useful if your desired product is the Harmala HCl as it is.
Separation of harmine and harmaline Freebase:
If you don't want to separate the freebases, simply skip ahead to adding sodium carbonate. This will force both alkaloids to crash out.
-Add crystals to pan and 200ml of tap or distilled water (pour through the filter which the crystals were recovered from to dissolve those stuck to the paper).
-Gently heat until everything is dissolved and filter into a jar through a coffee filter.
-Add 100ml of sodium bicarbonate solution (saturated at room temperature).
-Solution becomes slightly cloudy. Harmine begins to precipitate. More base solution can be added until no more precipitation is seen (it may take about 300ml total).
-Let solution settle for several hours then pour through coffee filter to collect harmine freebase.
-Rinse harmine 3x in the filter with cold tap water (as distilled water can be slightly acidic) to remove traces of sodium bicarbonate, then dry.
-Add sodium carbonate solution (saturated at room temperature) to the bicarb based tea. Pale harmaline freebase will crash out. Add more as needed (it may take 150ml this time).
-Let solution settle for several hours then pour through coffee filter to collect harmaline freebase.
-Rinse 3x in the filter with cold tap water then dry.
My yields: Harmine freebase: 1.9g. Harmaline freebase: 1.5g. Total 3.4% final yield after cleaning. Yield varies depending upon quality of seeds.
Notes:
I think a manske step is a good idea, and only one is necessary if everything was done correctly. Brennendes Wasser has shown some evidence that the insoluble remainder after adding acid is in fact just harmalas which won't dissolve for some unknown reason : Harmala extraction - unneccessary steps? . If this is the case, the dark insolubles could still reduce the effectiveness of a dose. In my opinion it does make sense to remove them. Further purification can be done to remove color, but if the product as pure as the tests have shown then it's more about cosmetics and will have little to no effect on dosage. That said, you can manske and base to your heart's content. For simplicity I haven't included such steps here. See The Tao of Rue Extraction or Harmalas Extraction and Separation Guide for info about this.
If you want to grow nice crystals but don't want to go back and forth with manske and base steps, you can do it as part of this method as a freebase. Simply add your base solutions very slowly over a much longer period of time and you will see small crystal clusters develop on the sides of the jar and on the surface of the solution. This is easy for harmine as the pH does not increase too rapidly with sodium bicarbonate.
I don't recommend adding sodium bicarbonate powder or oversaturated warm bicarbonate solution to a cooler harmala solution, as I have seen this cause excess sodium bicarbonate to flocculate as spongey masses that seem to trap dissolved particles, apparently including harmaline. Doing this after all the harmine had been exhausted, I noticed a color change from pale orange to a lighter yellow. Adding sodium carbonate after filtering the bicarbonate globs away did not precipitate anything as it should have. After redissolving the mass in another jar of water and adding sodium carbonate, harmaline did immediately precipitate.
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