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how to speed up mhrb filtration Options
 
Para
#1 Posted : 3/20/2012 5:23:49 PM

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Hi,

I'm doing an A/B using some finely powdered mhrb.
I'm using a vacuum filtration with a Buchner funnel, 135ml 70mm filter diameter.
The problem is the filtration is very very very very very slow due to the powder.
To filter 400ml I need 1 hour with 4 filter changes.

If I'll use a bigger Buchner funnel, like 560ml 110mm filter diameter, will the filtration
go faster due to bigger surface? I don't want to spend some extra money on a bigger funnel
and the speed to be the same.

Any other ideas on how to speed up the filtration of powdered mhrb, beside not using powdered mhrb or changing the filter more often?

thanks

 

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endlessness
#2 Posted : 3/20/2012 6:32:45 PM

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YOu shouldnt filter so finely, there's no need.. a funnel with a fat layer of loose cotton plug is more than enough.
 
Para
#3 Posted : 3/20/2012 6:51:16 PM

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won't I loose mhrb in the cotton by filtering this way?
and isn't fine filtering required before going forward with defating/basification ?
 
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#4 Posted : 3/20/2012 7:11:15 PM

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After you have acidified the MHRB the DMT should be released from the bark in to your aquious solution, so I dont see your concern about looseing your bark in the filter. Do you have another use for it? I've heard about the possibility of a second round of extractions with another solvent, but I havent played with that yet.

I use MHRB powder and a cotton t shirt in a glass powder funnel (much better than a coffee filter). Any leftover bark should settle in to your aquious layer when you get to the extraction part. If you are using a sep funnel some fine filtering with a coffee filter (or your vacu filter) after the cotton filter step will prevent any possible clogs. Also, i dont think there is any need to defat MHRB.
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Para
#5 Posted : 3/20/2012 7:33:28 PM

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I did 3 washes of the mhrb, 1h each, after each wash I filtered the solution.
So I needed to keep the mhrb for the next wash. If I filter with some cotton ball I think I'll loose some mhrb in it.

 
The Day Tripper
#6 Posted : 3/20/2012 8:05:10 PM

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My advice would be to put your water/bark in a container and let it decant. Pour off the top layer after its settled and then filter w/ the vac apparatus. You should be able to use one filter and have all the liquid fully filtered in under a minute w/ this method if you are careful to leave the sediment in the bottom of your container. Add more water to your bark, cook again, and repeat.

That way you won't have to filter the majority of your bark, and as long as you do 5+ pulls it will get all the alkaloids out. Filtering mhrb powder through anything is a pain in the ass imho. Decanting/settling then siphoning off is the easiest way to do acid pulls on bark powder. As long as you do alot of pulls it will get all the goods out. I've gotten %2+ yields on adenium bark w/ this method.
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endlessness
#7 Posted : 3/20/2012 8:13:57 PM

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Like daytripper said, decanting is good, very recommended!

Sometimes Ive done passing first through a metal strainer, then through t-shirt then through the cotton plug. Sometimes ive done using the top of the pot to help holding solids while pouring out the liquid. But definitely decanting makes things much easier.

Anyways I always like to filter it through cotton filter, and only very little powder will get trapped, most you will have decanted, and the bit that comes through will stay mostly on top of the cotton, which you can either pour back into your main boiling mimosa or just run a bit of warm water through the filter which should get the rest of the alkaloids.
 
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#8 Posted : 3/20/2012 8:17:55 PM

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I found that despite decating each pull separetly (30 minutes or so), an overnight decant still produced quite a bit of plant material.

Topic of interest.
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Para
#9 Posted : 3/20/2012 8:24:13 PM

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I didn't think of decanting prior to filtering, this is a very good idea, too bad I didn't found out about it before today
I'll keep in mind for the next time.

After the 3 washes and filtering after each wash I got 1 liter red cloudy liquid.
I'm trying now to filter again this liquid to make it more clear (I think vovin tek recommended this).
Unbelievable but the filtering of this liquid still takes ages, 140ml (one load in buchner funnel) need 20-30 minutes, then again I need to change the filter.

First day was full with acid washing and filtering.
 
Para
#10 Posted : 3/20/2012 9:05:00 PM

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and another question, is it absolutely necessary to have a clear acidic solution prior to basification ?

mine is cloudy, I cannot see at all through it.
 
Para
#11 Posted : 3/21/2012 8:37:52 AM

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I didn't boiled the mimosa, I kept it in a water bath around 70C (measured with a thermometer).
 
Para
#12 Posted : 3/21/2012 10:11:05 AM

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OK, so the list keep growing Smile, I'll keep in mind for the next extraction:
- heating bath at 50C max
- decanting prior to filtration
- filter first with some cotton, then with lab paper

Should I go further with the solution to basify it even if isn't completely clear?
It's cloudy, I cannot see at all through it.

Now I'm reducing it to a workable volume.
 
Para
#13 Posted : 3/21/2012 6:43:38 PM

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I finished the reduction and the liquid is totally black.
Is this normal?
Should I filter it again?
 
GratefulDad
#14 Posted : 3/21/2012 7:09:55 PM

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I only ever filter with a t-shirt. Works just fine. After 3-4 soaks and t-shirt filters, I put it in the fridge over night, and all the sediment settles, then I decant the liquid through a t-shirt filter one last time. When reduced, the liquid is very dark red, or almost black, and then it is fine to basify. If any tiny particles of bark are left in the solution, they will not be pulled into the solvent when the solution is made basic, so you don't have to filter it that thoroughly. Plenty of STB teks don't filter the bark at all, and they work just fine.
 
Para
#15 Posted : 3/21/2012 7:30:34 PM

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ok, then tomorrow will proceed with the lye and naphtha pulls Smile
 
Para
#16 Posted : 3/22/2012 2:43:57 PM

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I'm in deep trouble Smile))
I added 50ml naphtha to my basified solution then used a DIY magnetic stirrer (made from a computer fan) to mix the two phases.

All good for the mixing part, at high speeds the two layers are completely mixed so I was happy that naphtha is in intimate contact with the solution and will be able
to pool as much freebase as possible.

Then the surprise came when I need to run the 'magnetic stirrer' on low speeds to resolve the emulsion.
Is seems that the lowest speed it's capable of is still not low enough to have the effect of resolving the emulsions instead of mix them a bit.
Damn.
The clear naphtha phase is like 2mm height followed by 5-6mm emulsion.

I warmed it, let it rest, put it back on stirrer, more then 2mm clear naphtha I cannot get.
Tried to stir with a rod, make it worse.
Remain only to try to add more NaOH, but not sure is this will indeed change something.

 
ragabr
#17 Posted : 3/22/2012 2:55:57 PM

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More base, or adding kosher table salt, will get rid of the emulsion.
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GratefulDad
#18 Posted : 3/23/2012 2:01:58 AM

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More lye will do the trick for sure. Lye and patience. Don't bother with the stirrer, as I imagine the agitation isn't helping. With enough lye, separation usually happens within minutes, but if not, letting it sit overnight has always worked for me.
 
Para
#19 Posted : 3/23/2012 9:29:00 AM

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I added more lye, after my calculation the pH should be above 13.4 (someone said that this is the point where emulsions don't form anymore). I had 1L solution and the total lye added from the beginning was around 30g.

I let the solution undisturbed over night, the naphtha layer increase but there were no clear line between the two phases. Emulsion was like 2mm thick. So I took out the clear naphtha and put it in fridge.
Then I took the rest of the emulsion + some black solution, put it in a separate jar and added more water + lye (pH around 13). This addition tripled the total volume.
Big surprise !!!!!
Very quickly the emulsion disappear. I remember reading somewhere here that a too concentrated solution would make some impossible emulsions, so diluting it (with basic water of course) will solve them.

How can a 1L solution from 50g of mhrb can be too concentrated? I did and A/B and Noman tek recommends 1:15 ratio mhrb:water for an STB.
Very strange...

One more thing.
The fine line between the naphtha and black layer has a very fine white color. What can this be? DMT dropped out of naphtha?

 
GratefulDad
#20 Posted : 3/23/2012 4:25:51 PM

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I use 4-5 mls water, 1 gram of mhrb, and 1 gram of lye to extract with STB. I use much less lye with an a/b, though. works fine, and I think the excess water is overkill... If the solvent is very saturated and warm, DMT can drop out of the naphtha when it begins to cool down. I always just add lye, as well, not lye water. pH 13.5 will help break down emulsions, for sure.
 
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