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The Tao of Rue Extraction Options
 
plumsmooth
#41 Posted : 8/19/2011 1:05:54 AM

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I would just like to point out that if you have a scale you can be very accurate with your salting.
The Manske formula calls for 100 grams salt per liter 1000 ml water.
This is more than enough Salt to precipitate the Alkaloids.

Since water can hold 360 grams salt per liter:

Saturation is more than needed and can actually result in more salt contamination.
Once again even saturated cut in half is 30 more gram per liter than necessary...
 

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MelCat
#42 Posted : 8/19/2011 1:22:32 AM

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Ahh, I think I finally see what you're saying... Sometimes you gotta hit me with a brick.

So you create a salt solution with 100g of water per liter of water and add this to the saturated alkaloid solution?

From my experiments today it seems that if there is an excess of water, the crystals will grow better. Otherwise they just become a clump. I'm still waiting on everything to dry out so I'll probably report the yields tomorrow sometime.
Convert a melodic element into a rhythmic element...
 
MelCat
#43 Posted : 8/19/2011 6:11:47 PM

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So I weighed the dried alks and there was definitely a good bit of contamination.

The first test was around 700mg
The second and third tests were over a gram.

I decided to go ahead and clean up all of my harmine and try again at a later time.
Convert a melodic element into a rhythmic element...
 
plumsmooth
#44 Posted : 8/19/2011 7:44:22 PM

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I believe the simplest approach -- of course you need a scale --
is to re-dissolve your Freebase Harmalas in hot water/vinegar.
Measure the water, add 10g salt per 100 ml solution.
Done.
 
MelCat
#45 Posted : 8/19/2011 7:46:45 PM

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Yeah, that's pretty much what I did. Thanks for your help man. I'll update the Tek soon.
Convert a melodic element into a rhythmic element...
 
MelCat
#46 Posted : 8/28/2011 10:17:47 PM

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I think I've just about finished this tek. The only thing I plan to add is some more crystal porn and final yields.

If anyone would like to critique the Tek for me, I'd be highly appreciative.

I've read it so many times that most obvious errors are probably elusive to me.

Thank you everyone who has helped with this Tek, either directly or indirectly.

I love all of you <3
Convert a melodic element into a rhythmic element...
 
plumsmooth
#47 Posted : 8/29/2011 4:19:40 AM

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Quote:
Take a note of how many ml's you have. You'll take that same amount of fresh distilled water, boil it and saturate it with salt. Once it's completely saturated you want to filter it and add it to your alkaloid solution.


Why not change that to
Quote:
you'll take that same amount and add 20 grams salt per 100ml solution.


That would be the Manske standard because you're mixing that with its equivalent in volume.

Saturating, if done properly should be 36 grams per 100ml.

Half of that is still 18 grams of salt, 8 more grams than necessary as to the Manske formula.

Why use more salt than you need?

Anyway, that's my critique.
 
MelCat
#48 Posted : 8/29/2011 4:21:46 AM

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I put a note saying the Manske standard but I agree with your advice. I'll go ahead and change it so that there isn't any confusion.
Convert a melodic element into a rhythmic element...
 
Purges
#49 Posted : 9/22/2011 11:23:48 AM

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Ok, so all was going swimmingly until I added the salt (step 6). I made sure the solution was hot, by putting it in a hot water bath - all the alks looked like they couldn't wait to drop out of solution. All good there. I then added the salt and it went a bit weird - lots of floaty stuff on the top, and the alks all but disappeared. I left it for about 4 hrs, and not much change so I thought I had rue-ined (scuse the pun Razz) this run. I thought re-basifying might help the alks precipitate, so added some sodium carb (sodium bicarb cooked in oven for 90 mins on 180c) to the solution, which then fizzed profusely, and showed signs of precip, but then cleared up again?

What have I done wrong? Confused Think I may have just wasted 20 grams of Rue and a couple of days of my life?! Crying or very sad

Help please, really want to salvage this if possible!
Lose Control, Free My Soul, Break Me Open, Make Me Whole.
"DMT kicked my balls off" - od3
 
MelCat
#50 Posted : 9/22/2011 11:39:14 AM

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20g of rue? That's really not a lot to work with for an extraction. It's usually best to run with at least 50g.

I doubt you rue-ined it Razz The alks should still be in there somewhere.

You could add more sodium carb to finish basing the alks out. Depending on how much acid you used, it could take quite a bit. That's why I prefer to use lye until the final basing.

Since the alks are still in limbo, you could also add more vinegar to bring the ph back down. Once you've got a ph of around 4, you can add more salt to finish pushing the alks out of the solution.

I've been working with lots of variations of the manske procedure and if you've got too much water, the crystals won't grow. If you've got too much salt, you end up with a sludge. With the first couple of runs, it's better to have too much salt than too much water. The reason being, if you've got sludge, your alks are in there somewhere and can be cleaned up. If they stay in the water, there isn't much you can do with them.

If your brew is properly filtered and can make it through a coffee filter relatively easy, I'd recommend basing the alks the rest of the way and run the rest of the tek.

If it can't be filtered through a coffee filter, I'd add more vinegar, filter, reduce and add saturate with salt. This will ensure that your alks get pushed out. Then run the rest of the tek like normal.
Convert a melodic element into a rhythmic element...
 
Purges
#51 Posted : 9/22/2011 12:06:29 PM

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Thanks, think I'll try some more Lye, see if that does the trick, I'm not 100% I got the Sodium Carb right :S I'll get back to this thread and let you know how it goes, the first precip looked like I got a decent amount of alks, didn't want to use too much first time in case I got it wrong.

EDIT - more lYe seems to have done the trick, many thanks Very happy
Lose Control, Free My Soul, Break Me Open, Make Me Whole.
"DMT kicked my balls off" - od3
 
Purges
#52 Posted : 9/24/2011 5:24:47 PM

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Right, so the Lye precipitated a whole bunch of alks. I then decanted the remaining solution and redissolved the alks in some hot vinegar, followed shortly by salt water solution in the same ratio as the alk solution (Phlux's step) How long until the needles start forming? Its been about 10 hours now, and I can only see a bit of sediment at the bottom of the jar...

This Manske business is confusing me Confused
Lose Control, Free My Soul, Break Me Open, Make Me Whole.
"DMT kicked my balls off" - od3
 
MelCat
#53 Posted : 9/24/2011 6:54:14 PM

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10 Hours should have been enough time. I'd reheat the solution and add a bit more salt. If there isn't enough salt present, it won't "push" the alks out. They should start forming soon after the solution cools off. Definitely within two hours of everything cooling down. If you still don't have crystals forming after two hours, repeat the process with a bit more salt.
Convert a melodic element into a rhythmic element...
 
plumsmooth
#54 Posted : 9/24/2011 8:19:36 PM

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Once again there is no reason to eye salt content.
Follow the original Manske formula when attempting to Salt out the Alkaloids.

The recipe is as follows: 10 Grams Salt per 100 ml Solution.

Simple Enough...
 
astralspice
#55 Posted : 4/29/2012 11:15:40 PM

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First of all thans for this tek. But when I added the lye and let settle for a day I ended up with 3 layers. The alks crashed to the bottom and the middle layer is clear brown just like the pictures but the top layer is still cloudy. Should I add more lye to try to get the cloudy layer to crash out?
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MelCat
#56 Posted : 4/29/2012 11:32:45 PM

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I'm honestly not sure what to say about the top layer.

If you have a way to check the ph, I'd do that first, just to make sure it's at least 9 but not over 11.

If it's not, then I'd say add more lye solution. Also, you don't want to add the lye directly to the soup. You want to mix up a few grams of lye with water in separate container and while you're stirring the soup, slowly add the lye solution. When you crash the alks out the first time, there should be two distinct color changes that takes place.

If that doesn't work, take a pic and give some more info on exactly what you did so far and we'll figure out what went wrong.
Convert a melodic element into a rhythmic element...
 
astralspice
#57 Posted : 4/29/2012 11:43:24 PM

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yea, I wanted to take a pic but my batteries are dead. I added about 40 grams of lye/water solution to the quart jar which seemed to be enough at the time
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astralspice
#58 Posted : 4/30/2012 3:29:23 AM

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I gave the jar a lil swirl and the rest crashed out, it looks like I have a great yeild Very happy
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evil804
#59 Posted : 4/30/2012 3:36:22 AM

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i tried my first rue extraction using the Tao this week, currently have what looks to be 2-3 grams of light tan harmalas drying out after the final washings extracted from only 60G of starting material. Thanks so much for this tek, it really is the most thorough rue tek ive seen. I spent hours reading through every Rue tek i could find, and once i understood the chemistry involved it was clear this provided the best balance of yields/purity. i tweaked it a bit for my personal preferences.

1. i only did one manske. i planned to redissolve and perform another manske to further clean the harmalas but i noticed my harmalas already had lost most of the red color and appeared very clean after 1 salting. I did 11G of kosher salt for every 100 ml and it came out noticably salty, so +1 on going with 10G per 100 ml, seems like Manske got it perfect down to the last gram.

2. After removing HCL harmalas from the water i based my manske water and retrieved what looks like another 200-300mg of precipitates. in another thread, it was mentioned someone did this and had it analyzed and it was mostly harmine. I plan to add this into my next extraction right before i perform the manske step to retrieve any harmine and prevent the Vas family from making it into the final precipitates. might be worth mentioning this option in the tek, some of us like to get every last Mg of harmalas from our rue!

3. Be sure to collect all waste water and let it settle for a few days. most all of my solutions after basifying still had a slight cloudy consistency and yellow color. there is probably another few hundred Mg from the looks of it. slight layer of solids at the base of the gallon worth of wash water that was saved in a large jug.

4. Definitely do the speaker/subwoofer trick speed up precipitate seperation! i noticed a lot of harmalas would either float in a thin film on the surface or cling to the walls of the container if left still, but the slight vibrations from a speaker made everything settle.

ended up with 2.3 grams from 60 G. 3.8%, not bad!!!! and i still have yet to recover harmalas from the waste water, probably another 300-500 mg in there from looks of it, so i may have 4.5-5% total yield!



 
MelCat
#60 Posted : 4/30/2012 5:06:39 PM

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Great stuff man! I'll add your suggestions to the wiki this evening, thanks for adding them! Congrats on a successful extraction!

Also, if you hit the TARE button on your scale after you add the lid or add the lid before you turn it on, it will zero out so you don't have to any math to figure out your yield.

Edit: It looks pretty darn good but you could probably still clean it up a bit more if you were so inclined. There's really no need to except that the purer it is, the more potent it is per milligram. I don't mind the end result being a little tan but I just wanted to letcha know it's possible to get it pretty freakin' close to white if you put the extra time in.
Convert a melodic element into a rhythmic element...
 
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