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Help clarify the tao of rue extraction. I'm on the final base step Options
 
rbalzer
#1 Posted : 7/4/2015 3:32:56 AM
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(I greatly appreciate any help. this tek has been a tad tough and I'm really close)

Step 11 says do the exact same process as step 5 for the final basing. The part I'm hung up on is: After you've based, let it settle, and decanted off the basic water, step 5 says "you want to add some hot vinegar and water to your freebase alks to redissolve everything back into the solution as harmala acetates. Once your alkaloids are redissolved, filter out anything that won't dissolve. This is mostly plant matter and oils."

My question is: Is the vinegar vital to this step? Is the transformation into harmala acetate important in this final step?

And also, is the final filtering important?

Seems to me that I could just decant off the basic liquid and then start the washing procedure outlined in step 12

(It was hard to tell if the writer meant 'do step 5 to the letter' or 'do the same basing procedure as in step 5.'Pleased
 

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slewb
#2 Posted : 7/4/2015 4:28:58 AM

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If you've done enough manskes and filters, you can just wash your freebase with water to remove excess salt and sodium carbonate and you will be all set.

Honestly, for all practical applications I think the purity of harmala alkaloids is pretty unimportant as long as you remove all that comes out solid when the alkaloids are dissolved in vinegar at relatively low volume.
 
rbalzer
#3 Posted : 7/4/2015 6:45:09 AM
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thanks for the speedy reply.

maybe I should dissolve in vinegar one last time if filtering those solids is important? You make it sound like it removes the toxic stuff, and I seem to remember forgetting to filter at that point in the process
 
Jees
#4 Posted : 7/4/2015 11:17:07 AM

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To repeat the processes is to get cleaner end product.
To filter the acid solution is important, and I tend to run it trough same coffee filter several times because each time it becomes a finer filter and thus clearer liquid. If the filter gets clogged really fast then trow it away, it is when the filter gets dirty slowly that I start to reuse the filter. In the end it drips trough like only 1 or 2 drops / sec and then your end liquid is really clear translucent.
Happy cooking.
 
rbalzer
#5 Posted : 7/10/2015 7:30:40 PM
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So I got it all finished up (thanks again, to those who replied and the general community)

I'm a little concerned about the appearance of the final product though. I was expecting a brown needle-like crystaly yield. My yield is a white/offwhite/tan powder with a little tinge of brown in some spots.

Is this normal?
 
MelCat
#6 Posted : 7/10/2015 7:41:04 PM

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Yes, the salt form of harmala is the brown needle like crystals you were expecting. Freebase is the white/tan powder. Same stuff, just different forms.

There shouldn't be any brown mixed in though. You might want to do one more cleaning step so it's all white/off-white/tan.
Convert a melodic element into a rhythmic element...
 
rbalzer
#7 Posted : 7/10/2015 7:48:52 PM
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MelCat wrote:
Yes, the salt form of harmala is the brown needle like crystals you were expecting. Freebase is the white/tan powder. Same stuff, just different forms.

There shouldn't be any brown mixed in though. You might want to do one more cleaning step so it's all white/off-white/tan.

many thanks melcat! Perhaps I'll simply dissolve it in vinegar water and filter it. Or am I needing to re-base to clean it?

Looks like freebase is the desired form for smoking from what I just read. is this correct?
 
Metanoia
#8 Posted : 7/10/2015 8:07:37 PM

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It has to be freebase to be active when smoked, yes. The Hcl is better if you wanted to take them orally. It's just a matter of converting it back and forth from salt to base to clean it up. Like Melcat said, if there's still some brown in your freebase you need to clean it up a bit more.
 
rbalzer
#9 Posted : 7/11/2015 9:22:26 AM
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what would you recommend for cleaning it? Another manske? Another basification? or merely dissolve in vinegar and filter insolubles?
 
FLeP
#10 Posted : 7/12/2015 12:34:45 AM

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Repeat steps 5-8 just like it says in the tek.
 
Jees
#11 Posted : 7/12/2015 6:00:11 AM

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Metanoia wrote:
...Like Melcat said, if there's still some brown in your freebase you need to clean it up a bit more.

I've been doing many very successful rue extractions, 5 to 6 % yields, but this latest batch of rue is quite different. I really can't get past some brown in the FB, despite many A/B transitions, decanting the clear base liquid, and filtering the acid states trough really dense lab-paper with vacuum, and the yields are much less than used to.

There is a ton of FB material on the basings before manske, promising a lot, just a little brown, but then on the first manske it shows less needles than my other batches of rue. Sometimes it really is the seeds doing. I know I do nothing wrong or different in tec.

The rue was brought with me from a travel, from a local herbal shop. Seeds look quite okay at sight.
 
FLeP
#12 Posted : 7/12/2015 3:51:44 PM

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All the freebase I've bought off the internet was brown-light brown in color. Dissapointing but to be honest there was very little nausea. I haven't tried my own extracts, which are nearly white in color, for comparison.



 
Nitegazer
#13 Posted : 9/21/2015 12:01:40 PM

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Jees wrote:
Metanoia wrote:
...Like Melcat said, if there's still some brown in your freebase you need to clean it up a bit more.

I've been doing many very successful rue extractions, 5 to 6 % yields, but this latest batch of rue is quite different. I really can't get past some brown in the FB, despite many A/B transitions, decanting the clear base liquid, and filtering the acid states trough really dense lab-paper with vacuum, and the yields are much less than used to.

There is a ton of FB material on the basings before manske, promising a lot, just a little brown, but then on the first manske it shows less needles than my other batches of rue. Sometimes it really is the seeds doing. I know I do nothing wrong or different in tec.

The rue was brought with me from a travel, from a local herbal shop. Seeds look quite okay at sight.


Jees --

I've been reading a fair amount from this site and others on rue yeilds, and I think what happened is you extracted from seeds that were rich in harmalol. Several reports indicate typical yeilds of 2-3% harmine/harmaline, due to the majority of alkaloids being harmalol.

Harmalol is present in varied amounts in rue depending on season and other factors but can be half or more of all harmalas in rue. It is very soluble in water, so will not precipitate with harmine and harmaline in a manske.

Anyone Tried Harmalol?

 
Jees
#14 Posted : 9/21/2015 12:39:14 PM

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Thank you for the heads up NiteG.
When basifying a solution where all the manske needles are filtered out, one could expect to meet much of the FB harmalol then. I've found this FB does settle to bottom but could not be filtered easily because it merely showed as a slime rather than hard solid FB.
 
pitubo
#15 Posted : 9/21/2015 1:05:41 PM

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Nitegazer wrote:
Harmalol is present in varied amounts in rue depending on season and other factors but can be half or more of all harmalas in rue. It is very soluble in water, so will not precipitate with harmine and harmaline in a manske.

With some larger extractions, I got quite a bit of red crystals in the manske saltings. Would these be harmalol or harmol? The freebase would also be darker than usual, with a slight reddish/pink hue.

I also got a lot of red crystals on time when I tried to use HCl instead of NaCl in the salting, which worked initially, but when the filtered yellow crystals were drying, a lot turned red. When I read the original treatise by mr. Manske on his identification of the harmala alkaloids, I remember him writing that harmalol can be prepared from harmaline by boiling in concentrated hydrochloric acid.
 
Nitegazer
#16 Posted : 9/21/2015 2:21:45 PM

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pitubo wrote:
I also got a lot of red crystals on time when I tried to use HCl instead of NaCl in the salting, which worked initially, but when the filtered yellow crystals were drying, a lot turned red. When I read the original treatise by mr. Manske on his identification of the harmala alkaloids, I remember him writing that harmalol can be prepared from harmaline by boiling in concentrated hydrochloric acid.


This sounds a lot like 'harmala red' which was discussed frequently a few years back.

'harmala red' LC-MS analysis
 
pitubo
#17 Posted : 9/21/2015 2:45:36 PM

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Hmm, I'm not sure there is a single "red" substance.

Compare the red in the Syrian rue as a dye thread. It seems to be caused by alkaline conditions, oxygen and/or heat.

I've seen both reds and the color is different. The first is dark red, the other is bright.
 
Jees
#18 Posted : 9/21/2015 2:51:44 PM

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Pitubo, my batch of seeds with lowest yield was also chased by pink-red-ish hard to get rid of in the FB. And the needles after 2 manskes are also darker yellow but no red there.
 
pitubo
#19 Posted : 9/21/2015 4:37:42 PM

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I've had saltings with beatiful long yellow needles, interspersed with red needles. Sorry, no pics available. The red needles keep coming back after repeated saltings. I also sometimes get a crust of crystals that are intensely dark red, almost black accrued on the bottom of the precipitation jar. Apparently these are the first to drop out of solution. I am not sure if this is the same stuff as the brighter red needles, but at least the darker stuff can be separated out easier.

Another thing about the color of freebase: for all I know, harmaline freebase is white to off-white, but harmine is rather more tan. Perhaps repeated washes of freebase precipitations cause much of the harmine to be washed away, leaving mostly harmaline behind? The freebases are slightly soluble in pH 7 water, harmine more so than harmaline. Washing away substantial amounts of harmine would whiten the extract.
 
Nereus
#20 Posted : 9/22/2015 1:14:35 AM

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Quote:
When basifying a solution where all the manske needles are filtered out, one could expect to meet much of the FB harmalol then. I've found this FB does settle to bottom but could not be filtered easily because it merely showed as a slime rather than hard solid FB.


Did try this myself on few occasions with caapi as well as with rue as some users pointed out that per ex. during the manske step done on caapi vine some of the thh gets left behind due to it not bonding with the sodium ions.I tried it myself and based the leftover clear filtrate and obtained clouding after adding Na2CO3 to the salt water.I hardly could filter the precipitate but managed to in the end, dried it and saved it for a bioassay.I did not manage to try it out and see for my self if it was active but i recall snozz confirming an analysis about leftover harmalas that precipitate upon basing the salt solution are relatively pure harmaloids.
 
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