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P. harmala extraction with pictures / Update: microscopies of Xtals Options
 
Nicita
#1 Posted : 7/19/2012 11:29:04 PM

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After a small trial with 50g... An extraction with 150g using a pressurecooker. I documented the process with some pictures... have fun.



Step 1: Soak Rue in acetic acid.



Step 2: Add Water and boil for 2 hours.



Step 3: Make godd use of the time: Heat up your Vaporizer and take some good tokes,



Prepare some Herba the Maté, spiced up with some p. somniferum resin,



Make yourself a nice tomatoe chutney with lots of onions, garlic, chilis and other Spices. (Dont forget to use your Vaporizer und drink your Mate Wink )





Step 4: Strain your extract from your seeds and set up the presure cooker for another 2 hours.



Step 5: Filter and reduce your extract.



Step 6: Use blacklight to be amazed by the harmalas fluorescence.




Step 7: Extract until the water is only slightly coloured, keep on filtering and reducing the liquid.

Step 8: Basify with NaOH.



Step 9: Let it settle over night.

Step 10: Discard top layer.



Step 11: Heat it and redissolve with acetic acid and water if needed.




Step 12: Measure amount of liquid and add 10g of Salt to each 100ml of extract.



Step 13: Let alkaloids crystalize in the fridge over night.

Step 14: Smooth sharp edges of chipped funnel tip (don't ask... Embarrased )



Step 15: Filter your crystals and let them dry.



Still very impure... I really have to get myself a vacuum filter setup...
At the moment it would be pretty pointless to weight, because the crystals are still wet. The next step is to purify the crystals. I haven't decided yet, if I want to seperate harmin and harmalin.
Has someone experience with cleaning harmalas? What would be the best way to purify? Also constructive criticism and suggestions for improvement are always welcome.

The next days I will also add some good microscopic pictures of the crystals, so stay tuned. Wink
 

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cyantific
#2 Posted : 7/20/2012 6:32:52 AM

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Wash your alks with plain water a few times to remove some of the lye. Keep washing until the pH is around 8.0 Finish with a sodium carb wash.
 
endlessness
#3 Posted : 7/20/2012 7:43:52 AM

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I would just redissolve in warm water, filter with funnel/cotton filter, re-precipitate with base again, repeat whole process once more if desired. I like to keep alternating between base and salt precipitation.

cyantific, if you noticed, his last precipitation was harmala HCl, so he cant wash it with water or sodium carb
 
Nicita
#4 Posted : 7/26/2012 4:54:49 PM

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Thank you for the advice, I will try it that way. But it has to wait for some time now, much to do for university.

in the Meantime: Some microscopic images of the chrystals!






 
christian
#5 Posted : 7/26/2012 5:21:30 PM

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The top left has some african dogon houses with a mayan temple at the end,

the one on the right is Angkor Wat! Surprised
"Eat your vegetables and do as you're told, or you won't be going to the funfair!"
 
jamie
#6 Posted : 7/26/2012 5:27:04 PM

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Salvia divinorum expert | Skills: Plant growing, Ayahuasca brewing, Mushroom growingSenior Member | Skills: Plant growing, Ayahuasca brewing, Mushroom growing

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"cyantific, if you noticed, his last precipitation was harmala HCl, so he cant wash it with water or sodium carb"

Endless, he can wash it with water, I have done this many times with HCL. If you dissolve harmine/harmaline hcl in minimal ammount of hot water and then get it cold enough hcl crystal will precipitate again. You have to use minimal water and get the temp to go low enough. No salt added.
Long live the unwoke.
 
 
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