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Soxhlet tek Options
 
rumplestiltskin
#1 Posted : 9/29/2009 10:00:01 PM

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SWIM just got a new soxhlet and a CLLE (lighter than water) Cool but reading around the Nexus SWIM can't seem to find a detailed tek that uses this equipment. He knows how it's used and has a pretty firm grasp on what he'll be doing but if someone could chime in it would be much appreciated. SWIM would like to extract from mimosa, chacruna, or chaliponga and has access to Naptha, Heptane, DCM, and various forms of ISO.
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SuperRad
#2 Posted : 9/29/2009 10:14:42 PM
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I have a q, I'd like to ask in this thread as well, if using an acid wash, would HCl or Acetic be vinegar? Which is more volatile and thus likely to end up in the MHRB?
 
rumplestiltskin
#3 Posted : 9/29/2009 10:31:34 PM

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Acetic is vinegar, HCL is more volatile.
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Everybody's time come to be embraced by the light,
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SuperRad
#4 Posted : 9/30/2009 5:54:55 AM
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Hahaha I'm going to have to edit that post. Phenazepam is debilitating, even to simple activities such as typing. the way I had meant to phrase it was "is HCL or acetic preferreable?" Both are volatile, and you have told me HCl is more volatile. This might make me inclined to say that hcl is the best acid to use in a soxhlet as more hcl gas will condense and mix with the water, generating a lower pH.

But the question arises: is HCl TOO volatile? Will some be lost as gas, while the pH inside the Soxhlet chamber also drop too low?!

When on is boiling HCl/Acetic solutions what portion of the evaporate is water and what portion is acid? Will the figures change when the acid solution becomes saturated with the goodies from the sexhlet chamber.
 
timeloop
#5 Posted : 10/8/2009 5:49:59 AM

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SWIM just got a new condenser and would like to bump this thread to see if a decent soxhlet tek exists

 
rumplestiltskin
#6 Posted : 10/8/2009 11:00:09 PM

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Cool, what type of condenser did SWIY get? SWIM looked around at all the different styles and it seems the best type for soxhlet is the Allihn style that is typically sold with the extractor body, not sure why.

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timeloop
#7 Posted : 10/12/2009 8:49:29 AM

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SWIM was telling me that it was allihn condensor... but also has a freidrichs style condensor with a custom drip tube...

allihn seems to be the way to go.

Has SWIY had any success using the soxhlet and CLLE?
 
benzyme
#8 Posted : 10/12/2009 2:13:22 PM

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timeloop wrote:

allihn seems to be the way to go.


why's that?

the friedrich condensor has a greater cooling surface area
swim uses a friedrich, and prefers it over the allihn; has no problem with it whatsoever.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
timeloop
#9 Posted : 10/13/2009 5:41:50 AM

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in SWIMs situation the Allihn was cheaper and fits into the extractor without any adapters. Plus the friedrich SWIM has is a little strange as it has a unique drip tube...

I guess the extra surface area of the friedrich condensor would make it superior plus the spiral design is nice to look at Pleased

Benzyme you seem to be rather knowledgeable about the usage of soxhlets... do you reckon you could outline a quick tek for new soxhlet users to experiment with?

SWIMs ponderings are focussing on wheather to use ethanol to extract DMT-tannate(??... evap then bassify and pull with acetone...
or
Vine gar run in the soxhlet then standard a/b

or is there a better way to go?

SWIM is also looking to forward trying a batch of mushrooms with ethanol as soon as there is some free time Smile
 
rumplestiltskin
#10 Posted : 10/14/2009 10:01:26 PM

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timeloop wrote:
Benzyme you seem to be rather knowledgeable about the usage of soxhlets... do you reckon you could outline a quick tek for new soxhlet users to experiment with?

SWIMs ponderings are focussing on wheather to use ethanol to extract DMT-tannate(??... evap then bassify and pull with acetone...
or
Vinegar run in the soxhlet then standard a/b

or is there a better way to go?


SWIM's thoughts exactly! How 'bout it Benzyme, you da man!

SWIM hasn't received the glassware yet so he hasn't gotten started experimenting, soon though. He's been having trouble tracking down solvents with low boiling points for use in the boiling flasks. Any swimmers know if IPA or ethanol is at all miscible in heptane?
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benzyme
#11 Posted : 10/15/2009 1:15:12 AM

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they're not miscible at all; alkanes are hydrophobic, and alcohols can hydrogen-bond with water.

a soxhlet tek wouldn't be necessary because there's really not much you can mess up. just use enough alcohol (about 2/3 full) in the pot (round/flat bottom flask) so that it will effectively fill the extractor body to the top level of the siphon.

notes:
use powdered bark.
everclear would be a suitable solvent, though some have reported using IPA with some success. let the soxhlet run for several hours, about 6 - 10. when finished, perform an A/B on the alcoholic extraction to clean it up, as alcohol will pull plant sugars.

"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
timeloop
#12 Posted : 10/15/2009 7:53:57 AM

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sorry if this sounds like a rather stupid question... but can you please clarify the a/b on the alcoholic extraction stage? Does this mean to add acid directly to the alcoholic solution and then bassify and pull with non-polar solvent? If so which acid and solvent would you recommend?
or should all of the alcohol be evaporated or distilled(?) first?
 
benzyme
#13 Posted : 10/16/2009 1:02:29 AM

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timeloop wrote:
Does this mean to add acid directly to the alcoholic solution and then bassify and pull with non-polar solvent?


exactly.

dilute acetic acid (vinegar) works fine.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
rumplestiltskin
#14 Posted : 10/16/2009 3:41:33 AM

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benzyme wrote:
they're not miscible at all; alkanes are hydrophobic, and alcohols can hydrogen-bond with water.


Just what SWIM wanted to hear. So his plan is to use ethanol or IPA in the soxhlet to do the initial extraction on powdered bark. Should he add acid to the alcohol before extracting? Anywho, after running the soxhlet for a good long time he then plans on adding lye and switching over to the CLLE and using heptane to (hopefully) extract fairly pure DMT. Does this sound like it would work?
Good morning.... good afternoon.... goodnight,
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benzyme
#15 Posted : 10/16/2009 3:55:15 AM

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Cool
yep


definitely worth a shot. experimenting is half the fun.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
rumplestiltskin
#16 Posted : 10/16/2009 11:28:34 PM

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So should he add acid to the alcohol before extracting or no?
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benzyme
#17 Posted : 10/17/2009 12:30:35 AM

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i suppose he could

may take longer though, the b.p. of the sol'n will be higher than the alcohol but lower than the acid alone, respectively
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
timeloop
#18 Posted : 10/17/2009 5:13:09 AM

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how much acid? 1:1?
 
benzyme
#19 Posted : 10/19/2009 1:49:53 AM

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enough to drop the pH to 3 - 4
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
timeloop
#20 Posted : 10/19/2009 6:30:40 AM

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of course Pleased

SWIM dropped the ph meter into a brew and it no longer works, been having dificulty measuring PH recently... time to get another one
 
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