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Solvent very clear... Options
 
demitritimmers
#1 Posted : 5/19/2009 11:25:40 PM
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Hello everyone! Before I even ask any questions, I would just like to thank everyone who has contributed to this amazing forum... without the combined knowledge of everyone who has been a part of this website, extracting alkaloids at home would be much more difficult, even impossible for many!

On to my question... A good friend of mine has extracted approximately 2.8g of the good stuff from 200g MHRB using Noman's tek. I assume a lot of this weight is composed of impurities. The batch was actually split into two 100g batches, adding the leftover lye solution from the first batch with the second to collect any alkaloids that may have been left behind. He actually screwed it up initially, using only half as much water as is called for for the first batch. Once he realized what he had done, he corrected the amount of water for the second batch.

I described this process simply to give you a bit of my friend's history of extractions. He is now doing two separate 200g MHRB extractions, performing the same extraction process as last time (sans the water screw-up). He is currently at the point of collecting the organic naphtha layers and noticed that the solvent is almost entirely clear, even after letting the mixture sit for several hours (up to 12) between pulls and agitating frequently. This contrasts sharply with the bright yellow pulls from his first ever extraction(s) described in the paragraph above.

Is this something to be worried about? I know the yellower the solvent is, the more alkaloids that have been extracted... I'm not really sure what I should do at this point. Any advice? Thanks!
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Jorkest
#2 Posted : 5/19/2009 11:30:17 PM

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try heating your solution..
it's a sound
 
hedcase
#3 Posted : 5/19/2009 11:57:05 PM

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Jorkest wrote:
try heating your solution..

Worked for swim!
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threeleggedlion
#4 Posted : 5/23/2009 11:52:11 PM

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I waited for a day and got no yellow solvent. After a hot water bath it was loaded with color.
 
demitritimmers
#5 Posted : 5/25/2009 8:20:15 PM
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You guys rock, worked like a charm.

So does anyone have an idea of how hot the solution should be, and for how long the solvent should be allowed to sit with occasional agitation in order to get the best results? Is this a function of the volume of the solution or the dimensions of the container?
 
Jorkest
#6 Posted : 5/25/2009 8:25:33 PM

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well you dont want it to get any hotter than say...110F..but 100F should be fine..agitate it like this for say...one hour..and then decant/suck the still warm solvent..
it's a sound
 
demitritimmers
#7 Posted : 5/25/2009 8:37:59 PM
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That's the temp I figured it should be... why do you not want it to get any hotter than 110F?
 
threeleggedlion
#8 Posted : 5/25/2009 10:49:23 PM

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The solvent would extract too many fats and tannins.
 
Xstacy
#9 Posted : 5/26/2009 9:34:44 AM
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SWIM has only ever heated the naptha slightly but usually this isnt a problem as the lye+water creates a nice warm temp to begin with. SWIM also takes left over naptha and adds it back to the solution and rolls it over some. Never had a problem, maybe its how you agitate the jar?
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burnt
#10 Posted : 5/26/2009 10:13:45 AM

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Solvent doesn't always get yellow. It may get more yellow when concentrated.

If SWIY isn't getting anything after evap or free precip yea do the heat thing or increase the pH or mix better (gently to not create emulsion).
 
demitritimmers
#11 Posted : 5/26/2009 6:14:56 PM
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threeleggedlion wrote:
The solvent would extract too many fats and tannins.


Wouldn't that also mean it would extract more alkaloids? I assume what you're saying is there exists a point in the solvent temperature where the solvent will extract more fat than alkaloids...? (ie more fat than it's worth?)

My friends extractions have been going incredibly well, but any increase in efficiency would help. So, let's say we have a gallon milk jug containing 200g MHRB, 200g NaOH and 1500mL water. How long would one agitate this container for maximum extraction efficiency? I know the more surface area, the better, so an indefinitely long time would be best... how long do you guys usually agitate a solution of that volume?
 
burnt
#12 Posted : 5/26/2009 8:16:51 PM

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^^Well unless you don't mind plasticizers being in your non polar solvent (which wouldn't matter if you freeze precipitate) then SWIM wouldn't use milk jugs.

Anyway SWIM always uses glass for any plant extraction. But glass is expensive so SWIM understands most people don't have.

Quote:
That's the temp I figured it should be... why do you not want it to get any hotter than 110F?


Quote:

The solvent would extract too many fats and tannins.


SWIM has never had such a thing happen. But then again who knows.

When doing STB SWIM heats up hexane (which is more pure naptha so it shouldnt matter) until its all wavy and bubbly and then pours it over the basic solution which is being stirred in a large glass flask. SWIM then pours back and forth between another glass flask gently to make sure the solutions get a chance to mix. While SWIM is doing this SWIM keeps the solution on a hot plate to make sure it stays reasonably warm. SWIM never keeps track of the temperature.

What SWIM is trying to say in too many words is it doesn't really make a big difference. Just keep it warm. If it feels warm and its not burning its fine.

Quote:
How long would one agitate this container for maximum extraction efficiency? I know the more surface area, the better, so an indefinitely long time would be best... how long do you guys usually agitate a solution of that volume?


SWIM usually lets the bark sit in base for at least overnight. When SWIM does pulls he does it for a couple hours of mixing agitating warming and settling. Usually also leaves it overnight if he gets lazy that day.
 
threeleggedlion
#13 Posted : 5/26/2009 8:57:02 PM

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swim doesn't mind the yellow oily goo because it bunches together and stays away from the crystals. he shakes it and let's the solvent separate, and then mixes again. He waits 24 hours between each pull but isn't sure if this is necessary. he only got fats after his first pull as well.

Does the solvent even have to be yellow? Swim wants white crystals and all he gets out of the yellow solvent is yellow crystals..

burnt, after looking at the second pull there was no yellow goo, so maybe it wasn't the heat. Does your friend know why?
 
burnt
#14 Posted : 5/26/2009 9:05:22 PM

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Quote:
Does the solvent even have to be yellow? SWIM wants white crystals and all he gets out of the yellow solvent is yellow crystals..


No the solvent doesn't have to be yellow. SWIM sometimes only sees yellow when its really concentrated or not at all. SWIM also tends to wash his non polar solvent though with pH 10 water (with sodium carbonate as base) so SWIM believes that cleans out a lot of junk. Also SWIM uses pure hexane which is more selective.

Quote:
burnt, after looking at the second pull there was no yellow goo, so maybe it wasn't the heat. Does your friend know why?


Do you mean no spice or just no yellow impurties? If you mean no yellow impurities then thats a good thing. It means they probably all got pulled out in the first pull.

SWIM would always recommend using heat when doing STB with naptha or hexane. Even with other solvents like toluene or limonene. It improves the solubility of spice in all of the above.

But yes in a sense that means it will also improve the solubility of other gunk but that gunk can be removed 1. by doing a wash with slightly basic water 2. recrystallazing.
 
 
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