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Soxhlet tek Options
 
rumplestiltskin
#21 Posted : 10/21/2009 4:25:01 PM

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So it doesn't really matter whether SWIM adds acid to the alcohol before or after the soxhlet? Sorry, my friend has a thick skull...
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Crystalito
#22 Posted : 10/21/2009 6:00:55 PM
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Hmmmm ,from my understanding i think the alcohol is best if added before the soxhlet (that is in the flask with the solvent) if i get your question right.That way it might aid the extraction from the plant material by converting alkaloids to the respective salts while extracting.

Another idea that might or might not prove useful : One could measure the volume of the solvent to use,and calculate the amount of acid needed for the desired pH.Instead of adding the acid to the solvent flask ,could it be possible to wet with it the plant material in the thimble? This way the acid will start converting alkaloids into salts even before the condensed solvent starts extracting it.This way the first run might be quicker because of the low bp of the alcohol ,and subsequent ones could propably fall back to the original time when the first "wash" siphons back and brings the acid in the heating flask.

I think this could ensure a better contact of the acid with the plant material, and propably lower initial pH in the thible (soaked material with concentrated acid) vs subsequent runs (or runs with acid preadded to the solvent) which is going to be higher pH due to it being diluted.

 
rumplestiltskin
#23 Posted : 10/29/2009 2:50:38 AM

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Any swimmers have any info on the boiling point of DMT? It seems that traditional jungle aya is usually boiled long and hard and it never seems to affect the brew. Of course, they're typically using chacruna/chaliponga....
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soulfood
#24 Posted : 10/29/2009 2:59:18 AM

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I'm not sure what the state that DMT is in the raw plant matter, but use the fact that water boils at 100C as a guide.

It may be somewhere around 150, but that's just a wild guess.
 
rumplestiltskin
#25 Posted : 10/29/2009 11:08:18 PM

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^
For sure, SWIM is trying to stick with low boiling point solvents n his soxhlet, stuff under 100 C just to be on the safe side. So far acetone, IPA, and ethanol are being considered. He will add enough acid to bring the ph down around 4, probably vinegar. Then add base and pull. What would be best to pull with? He would like to use (hot) heptane and just pull straight DMT but SWIM is not sure that it's soluble enough in heptane. If so, what would be the best base to use?
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rumplestiltskin
#26 Posted : 10/29/2009 11:15:59 PM

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Also, in a lighter than water CLLE, what's to keep the condensate from simply floating up inside the dispersion tube instead of being (somehow) forced out the bottom and up to the top layer like it's supposed to. Is the short drop from the condenser (ie gravity) enough to get it out the tube and into the solution?
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rumplestiltskin
#27 Posted : 11/14/2009 4:16:27 PM

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Bump
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69ron
#28 Posted : 11/14/2009 11:39:56 PM

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rumplestiltskin wrote:
^
For sure, SWIM is trying to stick with low boiling point solvents n his soxhlet, stuff under 100 C just to be on the safe side. So far acetone, IPA, and ethanol are being considered. He will add enough acid to bring the ph down around 4, probably vinegar. Then add base and pull. What would be best to pull with? He would like to use (hot) heptane and just pull straight DMT but SWIM is not sure that it's soluble enough in heptane. If so, what would be the best base to use?


Don't use acetone. It's been shown to be very poor for extracting DMT from mimosa. Some DMT salts are not very soluble in acetone.
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69ron
#29 Posted : 11/14/2009 11:51:04 PM

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rumplestiltskin wrote:
Also, in a lighter than water CLLE, what's to keep the condensate from simply floating up inside the dispersion tube instead of being (somehow) forced out the bottom and up to the top layer like it's supposed to. Is the short drop from the condenser (ie gravity) enough to get it out the tube and into the solution?


As the condensate settles down in the dispersion tube it builds up weight and the weight of it eventually is greater than the weight of the water below, and this forces it down the tube and out through the water below.

You can test this out with a straw. Pour some naphtha, which is lighter than water, into a straw that’s sitting in some water. If the straw is tall enough, eventually the naphtha will start pushing the water out of the straw at the bottom as the naphtha builds up in the straw. If the straw isn’t tall enough it just overflows. How tall the straw needs to be depends on the difference in density of the two solvents.
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rumplestiltskin
#30 Posted : 11/16/2009 3:42:41 PM

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Thanks ron, that makes sense. So no acetone huh? What about IPA (70, 90, or 99%) for the acid soak, hexane for defat/pulls, and heptane for re-x?
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69ron
#31 Posted : 11/16/2009 4:06:57 PM

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Methanol or ethanol is better than IPA because they are more polar. But IPA works. SWIM has used IPA many times with chacruna in a Soxhlet and gets great DMT yields with that. Mimosa didn't seem to work as well, but maybe it was just weak mimosa.
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D_Juggz
#32 Posted : 12/21/2009 1:20:44 AM

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SWIM just finished an IPA extraction, was wondering what to use for the defat solvent? naptha?
69ron what do SWIY do once you have run IPA through the soxhlet and have the alcoholic green DMT solution?
from what i can tell:
IPA mixes with water
IPA mixes with naptha
how do you get the layers to separate?
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Attention All Shipping
#33 Posted : 12/21/2009 5:59:35 PM
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Been a while since I've been on this site so interesting to see this thread.
D_Juggz, let us know how the IPA soxhlet extraction goes. I've had poor experiences with using IPA in a soxhlet to pull mimosa. I've done STB & A/B with IPA - both 99% & 91% IPA which is what is recommended - but haven't had much luck at all. Hopefully you'll do better.
Naphta's probably as good as any other solvent for a defat after you've acidified. Naphta & IPA shouldn't mix but should form seperate layers.

You may've seen this thread before but its got a lot of useful info on it.
 
D_Juggz
#34 Posted : 12/22/2009 4:14:20 AM

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Ok so SWIM watered down the IPA to about 91%.
I found it boiled a bit easier that way, and it extracted the DMT like a dream from the Psychotria viridis dried, crushed leaves.
It was a very dark liquid once finished, SWIM was wondering if adding vinegar to the IPA would speed up the extraction?
After, SWIM added NaOH, that should make the DMT insoluble in polar solvents (water) but soluble in non-polar solvents (Shellite).
Anyway SWIM just wanted to see how much would be in 12g of leaves, which wasn't much. A decent defat is required because, there was a lot of excess oil when the naptha was evaporated off, smelt like DMT but swim discarded it. Will try again next year.
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voidwalker
#35 Posted : 3/18/2010 1:25:28 PM
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i am interested in a good soxhlet extraction tek for mimosa. can anyone provide some new info?
 
D_Juggz
#36 Posted : 3/25/2010 5:42:40 AM

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Good question voidwalker, SWIM is wondering the same thing. He is busy writing one on paper. Should we collaborate into a new thread?
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rumplestiltskin
#37 Posted : 3/25/2010 11:41:43 AM

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^
That would be awesome!
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Trickster
#38 Posted : 4/23/2010 3:12:51 PM

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rumplestiltskin wrote:
^
That would be awesome!


Any progress here?

SWIM did a fair amount of experimenting with IPA and is not impressed with its efficiency. Lots of oils, sugars and what not is pulled. Lots of cleaning is necessary and as a result poor yields - usually 50% of those of STB. Time-wise there is no advantage over STB.

Are there forum members that have experience with using different solvents in soxhlet? In particular with

- ethanol
- methanol
- acidified water.
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benzyme
#39 Posted : 4/23/2010 3:22:47 PM

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i thought you guys would have figured this out by now: alcoholic extractions are never selective.
they'll pull anything that can interact in h-bonding
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Trickster
#40 Posted : 4/23/2010 3:55:07 PM

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benzyme wrote:
i thought you guys would have figured this out by now: alcoholic extractions are never selective.
they'll pull anything that can interact in h-bonding


Thanks, benzyme,

It seems, SWIM is one of those who learns from her own mistakes onlySad .
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