Large Soxhlet extraction of 1KG MHRB in 100% Anhydrous enthanol

[noone]

Hello,

SWIM have recenlty purchased some lab gear and am trying my first extraction this week.

SWIM have pulverized the material with a 600watt soy bean grinder (works fast). SWIM then used a small wire sieve to strain out the fiberous material. Resulting in a fine powder which SWIM will weigh.

The sohxlet extractor is a 71/60 body which looks to hold about 1L of material. I have a 2L flat bottom flask with 24/40 neck sitting on a VWR 375 hotplat/stirrer. I do not have a stirrer for it and was wondering if anyone knows a decent method to make one? Magetized non reactive metal? Magnet in a teflon rod?

Ive got the condensor unit hooked to a pump into a cooler which I can put water and ice in sitting beside it.

SWIM does not want to proceed before they can figure out the rest of the best way to do this. Looking for ease or method and low time used. Should SWIM reduce or reclaim the solvent (can SWIM do this by removing the condensor and buying a distiller bulb?) and then start a normal stb or a/b? Can SWIM add some water and crash it out?

Sorry for my ignorance, keeping it to the nursery

 

[veda_sticks]

you can buy teflon coated magnetic stirrer bars, but for the life of me i cant remember where. Check some mycology suppliers. They supply those for use with liquid cultures on magnetic stir plates.

Im sure stirring rods only need to be ferris, not magnetic

 

[noone]

Fantastic. I don't know why I didn't look on ebay. Thought it would be more scarce that that I suppose.
As for the method. Can SWIM soxhlet the pulverized material in 100% alcohol for 4 hours (longer?), then reduce volume by 75% then wash? Starting with mhrb will SWIM need to defat?

Thanks!

 

[noone]

Can anyone point me in the rigth direction? Ive got all the equipment setup in my place and want to get a start on it to take some of this down before rent day.

 

[SuperRad]

May I ask why you're using ethanol? It's a good solvent, but I've read SWI-69ron explain that a solution of water and vinegar works well since the acetic acid evaporates alongside the water. You probably want to run this overnight... 10+ hrs (correct me if I'm wrong here).

Ideally, you can also use whatever solvent you plan to use to extract the freebase to do a defat of the MHRB in the Soxhlet before using your salt-solvent.

 

[noone]

I will re read that tek.

In a nutshell process with water and vin, then solvent, defat, then do the salt in the soxhlet as well? Wish there were more teks using this equipment.

 

[SuperRad]

Let's say you're planning on freebasing into naphtha (though you can replace this with any solvent that boils at a lower temp than water).

Set up the Soxhlet with naphtha and run for a few hours. Discard the naphtha.

Then set up the soxhlet again with water and vinegar and run overnight. Collect the vinegar water, basify using Lye or Sodium Carbonate and extract the freebase with naphtha, and you're done! Just freeze precip or evaporate the naphtha and you've got your goods.

ALTERNATELY:

Set up soxhlet with vinegar water and run overnight. Collect vinegar water. Defat in sep funnel with your solvent, discard solvent. Basify the vinegar water. Then transfer the freebase with a fresh batch of the same solvent. Discard vinegar water, and evaporate your solvent.

The advantage to this method is you can use ANY solvent since it doesn't need to boil like in a soxhlet, the disadvantage is that the defatting step makes for more work.

Do you have a continous liquid/liquid extractor or a separatory funnel?

 

[noone]

Hi and thanks for the post. I think I will try the first method. I have an extractor body and a ahlin condensor bulb unit above. Is that a liquid to liquid? Funnel is on the way.

SWIM will use ethnanol as the solvent for 4-6 hours. For 1kg ground how much solvent? Then evap and run again with water+vin 12 hours+.

Thanks again!

 

[SuperRad]

Is SWIY planning on ending up with the acetate salt of DMT? The reason I'm asking is once SWIY has the vinegar with the DMT-acetate in it, the only way to easily extract the freebase is to basify the solution and then extract with a NON-POLAR solvent like naptha, xylene, or d-limonene. Ethanol is a polar solvent and will just mix right into your vinegar solution and generally will be a pain.

One way to work around this would be to evaporate your vinegar solution leaving behind sticky tar-like DMT acetate (and other stuff), and THEN add Sodium Carbonate and water (just enough to get it wet) to freebase the DMT. Then dry again and dissolve in ethanol, then filter the ethanol (which will contain the freebase dmt) and evaporate away the ethanol.

Once again though, I would like to say that I would replace ethanol with a non-polar solvent. Ethanol will work, but it will be more of a hassle.

ALSO I do not think you can defat with ethanol!!!!! Because ethanol is polar, it will eventually absorb a serious amount of the natural DMT salt in the root bark.

If you're dead-set on using ethanol, don't bother using vinegar water, just run the soxhlet with ethanol for 24 hours and then evaporate the ethanol. Then freebase the leftover gunk with sodium carbonate like I mentioned above. Dissolve in ethanol and evaporate. This yield will be VERY impure.

Finally, here's a tek for using ethanol and acetone (available without suspicion from almost any hardware store):

Run the soxhlet with acetone for a few hours. DMT-tannate is not highly soluble in acetone, so the DMT loss should be minimal. Discard the acetone (or evap it to see what's left behind!)

Run the soxhlet for 24 hours with ethanol. Evaporate away the ethanol to reveal the DMT-tannate.

Freebase the DMT with sodium carbonate.

Use a small volume of acetone to solve away the freebase dmt (do this three times to get all the dmt out).

Evaporate the acetone and you're done.

 

[noone]

Thanks for all the help. SWIM pulled off two styles of extraction w/o using the soxhlet. A STB and a A/b vin/water lye. Drying the results of each. I think in the end swim will use a bulk stb method in milk jugs. Less work.

I guess I will fire the soxhelt up with some psilo and ethanol and see if that is more fruitfull. Thanks again!