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Just where is all my spice? Options
 
rave420
#1 Posted : 10/6/2010 8:02:25 PM
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Hello,

this is my first post, it took me a good 30 minutes of trying to post in the STB forum when i figured that i can't Laughing


someone recently ran an extraction on 2 lbs of Powdered MHRB.
First of all the bark was soaked in acidified water for a day, water was pulled off, more water added, x3
The collected acidified water was reduced under gentle boil to yield about 5 L of fluid.
All extractions and soaks were carried out in a 10L carboy.

The collected acidified wash was then basified until black, and pulls with Naptha were done. It yielded 2.7g's of spice, which is an awful yield imho, but i have the feeling i may not be done yet. I put the reduced and exhausted liquid aside and focused my attention on the remainder of the bark.

The remainder of the MHRB inside the 10 L carboy was then topped off with highly basified water. There were no sediments after basifying the rootbark.
This is where i screwed up. I thought i could add naphtha to this stuff that had the consistency of maple syrup, and then pull out the naphtha. No dice. As soon as i added naphtha to the basified carboy with MHRB in it (10L) it disappeared, and there was no layer formation observed over 2 days.

I approached the situation with logic, and after pouring a bit of the naphtha / basified rootbark remains into a jar i realized that the stuff was WAY too thick for any separation to occur. Quick fix, i added half volume naphtha / basified rootbark and plain water and over the next 12 hours a separation was observed.

Because i have never worked with a scaled up extraction like this i now realize i was not prepared to handle such a motherload of liquid in a safe and efficient manner. Either way, a trip to walmart acquired 12 2L jars, in which the rest of the syrup was then divided and diluted. Separation occurred just fine after dilution.

Naphtha was collected from all jars + original liquid and stuck in the freezer. evaporating some of this naphtha on a spoon yielded an oily film reminiscent of our beloved spice. There is about ONE liter of naphtha. 48 hours later, no crystals whatsoever have formed. There is a slight cloud formation to be observed when one blows gently on the surface of the liquid, just not nowhere near as strong as with a concentrated solution.

bottom line
1000g of bark, 2.7g yield so far = 0.27%
from what i assume there should be at least another gram or two in there somehow. Now i am wondering, if the gram or two (if anything) is dissolved in 1L of naphtha, is this too much naphtha for freeze precipitation to occur? Would i be better off evaporating the naphtha until i'm at like 200mls and then trying to freeze precipitate?

Any input is appreciated.

Thus far i have learned that i shall not attempt a large scale extraction unless i have proper vessels to do this in. I have done batches with 200g and 250g with great success and yields of 0.9 - 0.5%.
 

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athousandeyes
#2 Posted : 11/10/2010 10:11:05 PM

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Without reading the whole thing, you ruined it by pouring the water of fthe acid cook. I will read the whole post in a second, but seriously man, learn the chemistry behind this. The acid moves the DMT into WATER, then the base makes it able to be transferred over to the NP solvent.
NowHere.
 
athousandeyes
#3 Posted : 11/10/2010 10:12:39 PM

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oh my bad dude. Oh man, actually, this is a conundrum.
NowHere.
 
SHroomtroll
#4 Posted : 11/11/2010 9:17:52 PM

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Yeah i think you have to much naphta, evap at least 50% and see what happens.
 
Trickster
#5 Posted : 11/11/2010 10:43:10 PM

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SHroomtroll wrote:
Yeah i think you have to much naphta, evap at least 50% and see what happens.


That is a good suggestion.

I would slowly reduce naphta in a waterbath until it is cloudy when hot. That is a good indication that your solvent is supersaturated. Then proceed to slowly cool it to room temp. Then seal the jar and move it to the fridge, and so on.
Do not seek the truth, just drop your opinions.
 
 
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