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The Tao of Rue Extraction Options
 
endlessness
#81 Posted : 5/13/2012 5:06:01 PM

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Usually small needles are due to excess salt and/or having added it when its not totally boiling, so it precipitates quickly. Its better to let it cool slower too.

Redissolving manske salts in plain water should work just fine and not affect crystallization afterwards IME.
 

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astralspice
#82 Posted : 5/13/2012 5:25:26 PM

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endlessness wrote:
Usually small needles are due to excess salt and/or having added it when its not totally boiling, so it precipitates quickly. Its better to let it cool slower too.

Redissolving manske salts in plain water should work just fine and not affect crystallization afterwards IME.


Hmm thanks endlessness, I first tried with a minimal ammount of water (250ml) in which the alks formed right away. I was guessing it was because it cooled too soon so I added another 500ml of boiling water/salt solution and it took hours until the crystals formed but it was still the same ''snotty'' soup. Anyway I will take a third run at it and see what happens.
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endlessness
#83 Posted : 5/13/2012 7:11:39 PM

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dont use minimal amount of water, dissolve the alkaloids well in water and add exactly 100g salt per l of boiling harmala tea.
 
astralspice
#84 Posted : 5/17/2012 3:11:16 AM

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Ok well thanks to all for the help when I was in need you all seem like a good bunch!
Here it is....It turned out almost white and has to consistancy of say pulverized construction paper and very very fluffy. Not the greatest yield but I can sure make a nice pile of CHANGA with this 0.9g

astralspice attached the following image(s):
IMG00268-20120516-2136.jpg (383kb) downloaded 387 time(s).
IMG00269-20120516-2141.jpg (350kb) downloaded 385 time(s).
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MelCat
#85 Posted : 5/17/2012 3:14:56 AM

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Good stuff brother! Don't be worried about your yield... The more times you do the extraction process, the better your yields will be as you have a better idea of what to expect. Congrats!
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SaLiXeM
#86 Posted : 5/17/2012 7:51:12 PM

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I'm done with the basing process and now I have alks in the bottom of brew. Do I have to dissolve the alks with only vinegar or water+vinegar for the manske? I really love to have those big crystals!
 
MelCat
#87 Posted : 5/17/2012 8:02:50 PM

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Only hot vinegar.. Depending on the yield and how much base was used, it could take quite a bit to get everything dissolved. Heat definitely helps in this step.
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astralspice
#88 Posted : 5/18/2012 12:36:43 AM

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Typically, how many water washes would you do after the sodium carbonate wash? I did 2 filtering each through a coffee filter aprox 500ml each wash would that be enough?
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MelCat
#89 Posted : 5/18/2012 12:40:36 AM

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You basically want the solution to be pretty much clear once the alks settle. Once it looks kinda like the Remove Excess Salt, NaOH, etc portion of Gibran2's tek you should be good to go. https://wiki.dmt-nexus.m...lkaloid_Extraction_Guide
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SaLiXeM
#90 Posted : 5/19/2012 10:33:14 AM

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Finally finished my second extraction.I didn't get those beautiful needle like crystals but I did get lots more than my first extraction.Unfortunately I don't have measurement tools to know how much exactly I've got.



Thanks in advance Thumbs up
 
MelCat
#91 Posted : 5/19/2012 11:21:50 PM

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Congrats! That's the harmala hcl right?? If so, there might be some salt contamination in there so it's kinda hard to really judge how much you really have. If that's the freebase, you might want to clean it up a few more times Razz

The best way to use harmala salts are to start with a known amount of freebase and then perform the manske on those. That will allow you to know exactly how much salt is in the end product and from there you can dose accurately.

Good job so far though!
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SaLiXeM
#92 Posted : 5/19/2012 11:32:33 PM

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Melodic Catastrophe wrote:
Congrats! That's the harmala hcl right?? If so, there might be some salt contamination in there so it's kinda hard to really judge how much you really have. If that's the freebase, you might want to clean it up a few more times Razz

The best way to use harmala salts are to start with a known amount of freebase and then perform the manske on those. That will allow you to know exactly how much salt is in the end product and from there you can dose accurately.

Good job so far though!


Yes they are HCL.And yes It's not pure, there are some salts mixed with it Very happy Maybe next I could get more cleaner!
Thank you for the advice Pleased
 
jdubs
#93 Posted : 6/2/2012 3:11:03 PM

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G'argh woe! Woe is me!

OK, so I have been doing this tek for about the past week. It is my first extraction so please bear with me.

Overnight I had done my second manske, and in my vinegar there were some beautiful, golden fibreglass-like xtals growing. I was especially pleased to see this, as I thought I had screwed it all up. I am almost certainly not cracked up for this science lark.

Anyway, I had the xtals, they were beautiful. I then attempted washing them.

First wash went well. Ideal, the xtals settled to the bottom beautifully and I siphoned off the water.

The second wash dissolved all the xtals. G'argh!

What is going on?! This happened before and I was forced to re-base and re-manske. Please tell me I don't have to again.

Could it be there is so much sodium carbonate in the xtals that it is re-basing the water??? Or could the water here just be very alkaline??? Or were the golden xtaks all salt???

I also acid-washed the filters and thats a whole other nightmare that I will get to once these are sorted. I have saved all liquids from both base/manskes, so hopefully the alks are still in there somewhere.

Help. Please.

"Mama matrix most mysterious." James Joyce

"The next great step toward a planetary holism is the partial merging of the technologically transformed human world with the Archaic matrix of vegetable intelligence that is the Transcendent Other." Terence McKenna

Forgive, you'll live longer.
 
MelCat
#94 Posted : 6/2/2012 3:33:33 PM

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It sounds like you're right on track.

After you perform the manske, the alks are indeed in salt form (harmala hcl) so they are water soluble. I'm glad you kept the liquid from everything, so you shouldn't have lost too much.

Ideally, you want to re-base and re-manske a couple of times to get the purity where it needs to be.

From here, I'd suggest that you add the liquids together and base it again so all of your alks are in one place. When you base the alks with lye or sodium carbonate, they shouldn't be water soluble any more.

After this basing, if you'd like to purify your alks some more, you can redissolve them in some warm/hot vinegar or other acid solution, filter a few more times, manske the alks, redissolve in water/vinegar, filter a few more times and then do your final basing.

It's a pain in the butt but it's worth it in the end.

Good luck and don't give up!
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jdubs
#95 Posted : 6/2/2012 3:42:19 PM

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Ahhhh I see!

For some misguided reason, I have assumed you want the final product to be a salt, and you wash that.

I have already based/mansked a few times now, so whatever is in there shoud be pretty pure.

If the solutions have a fair amount of vinegar in them, they are fine to base right? The liquids are all pretty vinegary.

Any basing that I have done recently has been almost white, so that sounds good I guess.

Thank you kindly for your swift response, you have just saved my panicking unscientific mind.

Laughing
"Mama matrix most mysterious." James Joyce

"The next great step toward a planetary holism is the partial merging of the technologically transformed human world with the Archaic matrix of vegetable intelligence that is the Transcendent Other." Terence McKenna

Forgive, you'll live longer.
 
MelCat
#96 Posted : 6/2/2012 3:54:57 PM

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Yeah, the vinegary liquids shouldn't be a problem. Just make sure you add the base slow so nothing spills over when it reacts. Good luck!
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evil804
#97 Posted : 6/21/2012 7:47:05 PM

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trying out using fumarates instead acetic salts for the manske this time around, curious to see the results. First round of manske was with vinegar/acetate and got some nice spiked needles. I decanted leaving about 5 grams of harmalas, and based the water from that first manske and got a HUGE cloud of precips. Did a seperate vinegar manske on that, and got maybe another gram or so from the manske water precips. looks like most of the alks left after the first manske are mostly vas-family and probably some impurities. Still worth doing IMO to get those straggler harmalas. Added the 2 manske precipitations together, based out, washed with water 4X, and redissolved in fumaric acid saturated water. Just finished heating the fumarate harmala solution with salt, and am letting it cool now. Into the fridge overnight, and we'll see what comes out!


curious, in a fumaric acid manske, what salt form precips out? is it HCL or fumarate?
 
MelCat
#98 Posted : 6/21/2012 8:29:24 PM

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Weird coincidence... I just did pretty much the same thing last night. I dissolved some freebase harmalas into some FASW and then manske'd it. I didn't allow full crystal growth to take place so I based the excess harmala/salt solution. There was a good bit of really fluffy precipitation that fell out. I'm still in the process of rinsing that out.

I'll update the wiki soon. I'd like to try to collect all of the tips and experiments people have done and really optimize the tek as much as possible.

If you or anyone else has any tips, tricks or things you do differently, please list them here so we can make the Tao the best rue extraction guide on the net!

As for what precipitates out when using fumaric acid and salt, I have no idea, but it's worth checking into.

I wonder if there are there any solvents that we could use to test? Maybe there is one that harmala fumarate isn't soluble in but harmala hcl is.

Another possible alternative is mass spec but I don't know if that would work or not...
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evil804
#99 Posted : 6/21/2012 9:45:56 PM

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this manske/fumarate is only at room temp for 3 hours, and already forming TONS of gorgeous crystals! definitely a distinct formation compared to the usual needles you get with vinegar manske (HCL). I tried but failed to get a picture of the crystals on the bottom, they have a dense solid golden center with hairs stemming off them, much like the center of a single dandelion seed head.



edit - got a semi decent pick of the dandelion like formations, hard to see the detail with my cheap camera, but gives an idea of the crystal formation.








 
MelCat
#100 Posted : 6/21/2012 9:47:51 PM

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Beautiful work!

I need to start working with fumarates more.
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