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Mhrb Soxhlet powder or shredded? Options
 
Kkvguitarist
#1 Posted : 12/30/2017 8:31:49 PM
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So my soxhlet is onnits way, gonna take a while to get here, but im reading every possible text on using a soxhlet and im trying to decide whether to order prepowdered or shredded. The powdered obviously gives better surface area and possibly quicker extraction, im trying to understand the best method for this. I beleive in the other nexus thread they are saying that POWDERED mhrb used with alcohol prevents clogging, but i want to make sure this is what they are saying. Also my previous extractions included zinc in the acidic phase inorder to de oxidize the dmt oxide, does the alcohol also extract the dmt oxide so i could still use this step with the acidification, or will alcohol leave the dmt oxide still in the bark? I ordered a 500ml soxhlet, how much material (grams) can i fit in a soxhlet this size? I know this is a multi topic thread but these are the questions i have come up with. Any help is appreciated!!
 

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Ulim
#2 Posted : 1/1/2018 10:06:26 PM

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well ofc the soxhlet will fit more powder than shredds
Both shredds and powder can clog the soxhlet so its a good idea to use some kind of filter to keep solids from going into the tube that sucks out the solvent.
You can use some filter to wrap the powder or you can place some filter like cotton over the hole making sure it still sucks over the solvent.
You want to make sure the solvent gets sucked out the rest is not really important.
So you can powder for max yield and efficency if you make sure it does not clog.
 
downwardsfromzero
#3 Posted : 1/3/2018 1:52:00 AM

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Cellulose Soxhlet thimbles are available to help prevent clogging. Quite a good idea if you've got the money for them. Makes it far easier to clean than just the cotton plug over the drain hole, at the expense of maximum extraction amount.




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Forestwalker
#4 Posted : 1/3/2018 2:23:05 AM

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, powder , surface area and yield will be better ,
 
antares
#5 Posted : 1/3/2018 12:51:14 PM

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Powder forms a gooey mass that will clog all but the coarsest of filters. Even shredded bark contains enough powder to clog cotton ball filters completely. It was one of the reasons I screwed up my first extraction. My suggestion would be to soak overnight in acid and filter with a coarse tea strainer to remove the powder from the shredded bark and then soxhlet the shredded bark.

While your soxhlet is doing its thing, do an acid boil on the sludge you have collected and let stand overnight then decant rather than filter. This is the first lesson I learnt from my failed extraction.

The second lesson I learnt was to make sure the naptha is at the same temperature or warmer than the bark extract. If it is cold, it forms a snot like blob that doesn't seem to pull the spice out very effectively. This was my biggest reason for failure.

Thirdly, make sure you have enough privacy. I nearly got busted by the wife and inlaws returning home earlier than anticipated and I had to pour all the stuff apart from two naptha pulls down the drain. The naptha hasn't yielded anything so far eventhough my extract had a very strong new shoe smell on basification.

Good luck with your extraction.
 
blue.magic
#6 Posted : 1/3/2018 7:52:48 PM

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antares wrote:
My suggestion would be to soak overnight in acid and filter with a coarse tea strainer to remove the powder from the shredded bark and then soxhlet the shredded bark.


This is actually a good idea. Simply soak the the bark in a solvent of choice overnight, then strain the water with coarse filter and transfer to Soxhlet for further extraction.

I naver experienced snot formation unless I heated the bark over 80 degrees centigrade. Maybe that also depends on acid used.
 
antares
#7 Posted : 1/3/2018 9:29:56 PM

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blue.magic wrote:

I naver experienced snot formation unless I heated the bark over 80 degrees centigrade. Maybe that also depends on acid used.


I don't want to derail Kkvguitarist's thread but I guess every bit of information will help.
My extract was at about 42C and the naptha was between 3C-9C. I used acetic acid and the bark was never boiled. Just buzzed in a 150W ultrasound cleaner for 20 min per extraction. The kitchen reeked of shoe shop and there were clouds of white precipitate on basification, so I am reasonably confident that there was spice in the mix.

The snot formed on mixing the naptha gently and it took a few hours to breakdown into naptha and a very small amount of aqueous stuff. I presumed that at that temperature difference, surface tension and density were doing funny things.
 
Kkvguitarist
#8 Posted : 1/4/2018 11:38:36 PM
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Ok, so i have 2 kilos of finely powdered mhrb comin, im plannin on doing a 99%iso run with it, dehydrating into a brick or whatever then rehydrating, acidifying, addind zinc dust, letting that cook for a bit, filter, basify then naptha pulls. Im planning on doing all pulls at room temp, trying to get as clean a product as possible, ive used heptane in the past just to clean, may do again, but as i do my pulls it goes directly into acidified water, the naptha is cleaned, then reused. Then this solution is basified, use either naptha or heptane, havent decided which yet, pull, reduce, freeze precipitate.

Im under the impression that using the 99 iso in the soxhlet helps it to not clog. Acidified antthing clogs it, but alcohol runs through. Any other views on this or my method?
 
downwardsfromzero
#9 Posted : 1/4/2018 11:41:50 PM

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I don't really see the point of zinc dust at this stage. Have you even tried it before?




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Kkvguitarist
#10 Posted : 1/4/2018 11:55:38 PM
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I have done the zinc once before, my thinking is that the alcohol will also pull the dmt oxide, and id like to get it back to dmt freebase, i ordered the bark.as a powder so the oxidation is definantly a factor. Should i acidify and zinc before running the extraction? Will alcohol not pull dmt oxide?
 
downwardsfromzero
#11 Posted : 1/5/2018 12:15:13 AM

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Were you saying you'd be doing the reduction on the results of an extract? Because that would certainly be better than mixing the zinc dust with the bark. It was easy to misread your post as saying the latter.

The cleaner the extract your treating with the zinc, the less random crud you'll have to deal with after. Basifying the crude iso extract and pulling with hot naphtha would pull the dmt and the oxide. Pull that back into HCl then add the zinc. That would be much tidier.

So you're aiming to get 40g of pure white crystals or something?

People would general recommend pulling in several smaller batches, I'm guessing you won't get all 2kg into the soxhlet at once?




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Kkvguitarist
#12 Posted : 1/5/2018 3:32:54 AM
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Lol oh god no 2kilo soxhlet... splooge.. yes extract with iso then do the zinc reduction on the extract then basify then pull with naptha. I have never been able to get more than 10 grams per kilo and its always yellow i can usually clean it up to very light fluffy almost white, but im thinking of just doing as many pulls necessary at room temp to get a cleaner product from the get go. I dont like "cleaning" after crystalizing, you can actually see the loss when you do it. I do a semi clean before crystalizing, i basically do an a/b/a/b ill be doing that from an iso extract this time. Im hoping to increase yield with this method and quality. Me personally i like making enhanced leaf, i call it changa, inknow its not technically changa but i like doing 50%dmt 50%passionflower.i go on 4 hour journeys with it and it never lets me down.

My biggest concerns are these:
Soxhlet getting clogged -solution- use straight 99% iso
Dmt oxide -solution- zinc reduction after iso pull and evap.
Im hoping im understanding the alcohol method correctly in that it drains easier and doesnt clog like acidic solutions.
 
Kkvguitarist
#13 Posted : 1/8/2018 6:36:54 PM
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So an update. Everything will be arriving this week. I am going to keep this community as informed as possible on everything. I am thinking of either making a picture tek, or maybe a video after i figure out the best method that works on powder without any clogging, and with nest possible yield. I am doing the acidic zinc reduction on the alcohol cake, i MIGHT do a side by side on 100g without zinc and 100g with zinc to see the quality and weight difference. If anyone could update me on the most recent a/b ph levels i would appreciate it. From what i understand the smaller the swing in ph the better product yielded, im thinking of going to ph 4, zinc reduction, filter very very very well, then to ph 11 for the pulls. All of this at room temp. I will premix lye and water, allow it to cool, then add to acidic solution.i beleive this will also yield a cleaner product. Any and all input is appreciated!!
 
antares
#14 Posted : 1/8/2018 6:49:18 PM

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I presume you have already studied Trickster's thread from 2010. There are some suggestions for PH ranges in it.
https://www.dmt-nexus.me...aspx?g=posts&t=13815
 
blue.magic
#15 Posted : 1/9/2018 6:57:28 AM

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Kkvguitarist wrote:
So an update. Everything will be arriving this week. I am going to keep this community as informed as possible on everything. I am thinking of either making a picture tek, or maybe a video after i figure out the best method that works on powder without any clogging, and with nest possible yield. I am doing the acidic zinc reduction on the alcohol cake, i MIGHT do a side by side on 100g without zinc and 100g with zinc to see the quality and weight difference. If anyone could update me on the most recent a/b ph levels i would appreciate it. From what i understand the smaller the swing in ph the better product yielded, im thinking of going to ph 4, zinc reduction, filter very very very well, then to ph 11 for the pulls. All of this at room temp. I will premix lye and water, allow it to cool, then add to acidic solution.i beleive this will also yield a cleaner product. Any and all input is appreciated!!


Thumbs up. I also plan pretty much the same process you describe.

As for the pH swing, Trickster notes:

Trickster wrote:
herefore, for an efficient A/B extraction it would have been sufficient to switch pH from 6.68 to 10.68.


To which benzyme replies:

benzyme wrote:
don't be afraid to exceed that range, extend it to 5 and 11.
by my calculations, DMT is 100% protonated at pH 5.2.


It's an overall interesting thread. Culminating in a complete Soxhlet tek from Trickster. Can't wait to try it!

You may also pre-soak your material in a warm/hot alcohol prior to Soxhlation. This will save you a few cycles.
 
Kkvguitarist
#16 Posted : 1/11/2018 7:31:55 AM
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Yes i am presoaking all of my bark powder in alcohol prior to the soxhlet, another thing i didnt mention but its whatbi figured, its hard to get alcoholnover 151 here, buuut with a soxlet, couldnt i theoretically put 151 everclear in and heat it up where alcohol evaps but water doesnt then condense in the condenser collect in the soxhlet and collect before reflux? Then use this high proof (95.7% or whatever the highest you can get with distilling) to extract the mhrb? From my understanding iso doesnt work as well as ethyl. And the high water content of 151 makes for slow evap. So even if im doing a zinc acid reduction 5.0 is where i want it at? And alot they are calling for heptane, i have naptha on hand, at room temp and in small amounts ive seen naptha work to get white crystals. If im doing all this should i just jump for the heptane or will naptha get it just as clean?

I am trying all room temp this time after the soxhlet. After the acid zinc reduction i am minimizing oxygen contact and heat to prevent it from re-oxidizing.
 
Kkvguitarist
#17 Posted : 1/11/2018 7:36:25 AM
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Oh and another quick question, a few posts up he said 40mg of pure white crystals. My heart would stop if i got that kind of yield. Does that sound possible to anyone? My yields with a kilo are in the 10 gram range. And i usually pull hot and get a light yellow,--- which was my intention at the time--- with the soxhlet and 2 kilos does anyone here think 40g of white lovely rocketfuel is possible??
 
downwardsfromzero
#18 Posted : 1/11/2018 8:25:43 PM

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Well, you could use the soxhlet glassware for a distillation, especially if it has a stopcock on the body to allow draining off of the solvent, although using the correct glassware would be (far) easier - particularly if your soxhlet extractor doesn't have a stopcock.

Having somewhere to put a thermometer into the vapour stream would also be rather useful.

Treat yourself to a few bits of new glassware Thumbs up

(Do you have a pic of your soxhlet setup?)


"Mr. Natural says - always use the right tool for the job!" - R. Crumb


Quote:
with the soxhlet and 2 kilos does anyone here think 40g of white lovely rocketfuel is possible??

With a bit of patience and the right bark you'd be seeing that from a combined series of STB extractions, for sure. So, why not?




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Kkvguitarist
#19 Posted : 1/12/2018 10:34:27 PM
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Soxhlet has arrived,, 500ml its bigger than i pictured it. Im so excited to get workin, now i just need my bark. Im psyched. Only thing is my lab stand clamps are too small. Im gonna need a new stand or a new way to hold ot securely while it operates. Any ideas? My bark supplier takes a while to actually ship but its always worth the wait. Psyched!
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20180112_140730.jpg (1,212kb) downloaded 85 time(s).
 
antares
#20 Posted : 1/12/2018 10:49:55 PM

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why not rubber-band it to your small clamps. I assume you will be using a keck clip between the flask and soxhlet.
 
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