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Switching ratios? Options
 
dooby
#1 Posted : 11/17/2013 10:03:21 AM

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Hello,

As a rule of thumb, if extracting 50 gr. of mhrb one would do 50 ml. pulls and do 5 of them, totalling 250 ml. for 50 gr. of bark.

Due to some chemical law regarding "equilibrium" there will always be some alkaloids left behind in the basic solution...

Would the equilibrium be affected if one would have, let's say 5 l. of solvent and add the basic solution to it dropwise? After separation and decanting one would salt the alkaloids out of the solvent so it wouldn't matter that an excess of solvent was used...

If this would be beneficial to yields I wouldn't mind giving it a try... The smaller the drops the better, perhaps agitation of the solvent, have solvent in as tall and narrow a container as possible... Due to the excess of solvent I think applying heat would be redundant, thus pulling less impurities...

Any thoughts?

PLUR

PS As the basic solution is added the volume ratio of solvent/basic solution changes thus maybe affecting the equilibrium so perhaps using a vessel with a tap or valve at the bottom so basic solution can be decanted at the same time as being added (once a layer of basic solution has formed on the bottom of the vessel)

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downwardsfromzero
#2 Posted : 11/18/2013 12:08:40 AM

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Liquid/liquid extraction equipment uses less solvent but has the overall effect of some of what you've been thinking about.

On left is for lighter than water solvents, heavier than water on right. Some kind of condenser is fitted on top. They've made it deliberately a bit unclear so it's hard to copy a few crucial bits at the top, I think.

There's probably some way of mocking up a similar setup at home if you don't want to spend hundreds of currency units on a brand new piece of laboratory apparatus...
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Du57mi73
#3 Posted : 11/18/2013 2:12:57 AM

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I like this idea.
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dooby
#4 Posted : 11/21/2013 4:14:07 PM

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I'm preparing for an experiment - due to restrictions in space, time and glassware this will not include a side-by-side comparison except the fact that it will be the same bark as my latest extraction...

I plan on the following...
1...prepare basic soup...
2 do wash of 50 ml of basic solution in 200 ml of warm naphtha
3 after separation/decanting salt naphtha in vinegar x3 (50 ml of vinegar per jar, 3 jars)
4 re-use naphtha, repeat steps 2-3
5 add NaOH and NaCl to each jar of vinegar
6 pull twice with warm naphtha from each jar of basefied vinegar - don't combine pulls from different jars
7 evap naphtha - compare results to establish usefulness of second and third salting
8 if yield is below par repeat steps 2-7

The amount of mhrb/basic soup to be processed this way will be relative to the amount of dmt-acetate that can be dissolved in the amounts of vinegar to be used (with a hypothetical 3% yield in mind)

Any questions or comments before I put this plan into action?
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Infundibulum
#5 Posted : 11/22/2013 10:28:51 AM

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dooby wrote:
Any questions or comments before I put this plan into action?

Sounds like complete waste of timeSmile

You cannot get out of bark more than there is inside in the first place. You can do all sorts of tricks and fiddle with rations here and there, but in essence (provided that the pH is high enough) you can get everything out by doing more pulls and/or using a better solvent than naphtha (like xylene, toluene, limonene, DCM, diethyl ether). Addition of salt may, arguably of course, help getting the most out especially if a poor solvent like naphtha is used.

Yet, nothing beats in simplicity doing a couple of extra pulls with a stronger solvent if you think that there is more to be extracted from the basic soup.




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