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Shades of Spice Options
 
frinj
#1 Posted : 6/21/2010 12:08:25 AM
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Here are some extraction results:





I found it interesting how I got these varied shades, from pure white to cocoa powder. But not yellow.

On the far left is a small pure white pile that is hard to see, either due to the flash or the white background.

 

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slayed
#2 Posted : 6/21/2010 4:40:19 AM

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So what did you do different for each pile? or did they just progressively come out darker?
 
gammagore
#3 Posted : 6/21/2010 9:32:01 AM

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Was this extraction done on the same bark? or did you use different extraction teks? That pile of "cocoa powder" looks dirty. Did you wash any of the piles?
 
frinj
#4 Posted : 6/21/2010 5:57:21 PM
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Okay, I'll try to break down how I got these. There are seven piles total -- six along the bottom and one in the upper middle. They are all from the same MHRB (pre-powdered).

The second pile from the left (second-lightest overall, nearly white) is what I got from an initial extraction run on 20g of MHRB. I made some mistakes, did not have good tools, was somewhat impatient, and had trouble working with the small amount of naptha (siphoning / decanting it cleanly). Hence the low yield.

The other six other piles are from 100g of the same MHRB. I did five pulls total on this extraction. The first pull was the pure white (bottom, very far left, hard to see, about 20mg). The second pull was the darkest (far right). The third pull was the next darkest (fifth along the bottom). The fourth pull was the third along the bottom. The fifth pull was the fourth along the bottom. So from the second to fourth pulls, the pulls were getting progressively lighter and then the fifth pull then went a bit darker again.

Each pull from the 100g MHRB was separately freeze-precipitated for 8-24 hours, then the excess naptha was filtered off the naptha into a "common" jar and the remaining crystals were dried. Ultimately, that "common" jar held the naptha run-off from all five pulls on the 100g of MHRB, and was a yellow urine color. I left this jar to freeze for another 48 hours, resulting in the pile of crystals along the top (which I think as sort of a combination of all the five pulls, and you can see the shade is in the middle). The naptha that was still remaining in the common jar was put in a glass dish for partial evaporation, and is still there.

Each of these pulls was cleaned according to Whatcha's TEK -- two sodium carbonate washes, one water wash, and an epsom salt wash after pulling and before freeze-precipitation. I had the use of a separatory funnel, too, for each of these pulls. So I expected to be getting a relatively pure result.

The two main differences between each pull -- apart from the order of the pulls -- was length of time each pull sat in the mother jug before being separated, and the use of a heat bath. For the last three pulls, I put the mother jug in a pot of very hot water after applying the naptha and let it sit there for 1 to 3 hours. For the second pull -- the darkest -- the naptha was in the mother jug for almost 2 days and I gave it a periodic heat bath in the sink (I'd get home from work, throw the jug into a sink full of hot water for a couple hours, then put it back on a shelf to deal with later). Heat was also only briefly applied to the first pull (the cleanest) after I first put the naptha in, at which time I put the mother jug in a sink of hot water for a couple hours, then set it on a shelf and separated it the next day.

So application of heat was a bit spotty, and the length of time each pull sat in the mother jug was a product of my other obligations and schedule, rather than any specific plan. Otherwise they were all pretty similar. It's interesting that those pulls that sat in the hottest heat bath for the entire time they were in the mother jug did NOT turn out darkest. I'm also still perplexed by how clean the first pull came out compared to all the rest, though I'm guessing it has to do with using the least heat with that pull (since the naptha pull is more selective at room temp, as I understand it).

I don't know if this could have any effect, but the darkest pull was put on a brownish opaque glass baking dish for freeze precipitation. I cannot imagine anything would have leeched off of the glass, but I'm no chemist (the glass shows no sign of color leeching off). A more likely culprit is that, on the second (darkest) pull, I failed to rinse out my separatory funnel between the time I used it to separate the naptha from the MHRB solution, and the time I used it to separate the various washes from the naptha. I think this means that some MHRB residue could have been left on the inside of the funnel and could have through that way.

I plan to recrystalize all but the lightest 2-3 piles with heptane.
 
sleeper
#5 Posted : 6/22/2010 7:32:31 AM
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When I add periodic heat (jug in near-boiling crock pot until contents are too hot to hold jug anymore), I don't get any change at all in the coloration...your differences in yield color confuse me!
 
frinj
#6 Posted : 6/24/2010 9:07:15 PM
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I have a few theories, but I really don't know the answer.

One thought I had is that if MHRB is pre-powdered TOO FINELY, then some plant material may get trapped in the naptha layer and pass through the washes to discoolor the final product. I don't know if that makes sense or not.

Another thought I had was that this might be related to using tap water rather than distilled water. I don't know how much of a difference that may make.

Finally, I wonder if these variations can be attributable to things like how the containers were washed. I mean, obviously laboratories have very rigid sterilization protocols. In my kitchen, I generally use dish soap and hot water, but jars sitting around may get a bit of dust, or may have some unseen soap residue, etc. Again, I do not know if this can have a significant enough effect to cause the discoloration I've experienced.

Well, I'm still leaning toward the notion that somehow MRHB plant material got into the post-wash naptha solution that I then freeze precipitated.

I'm just hoping it will come out with recrystallization, as I've read some posts suggesting this kind of discoloration can only be cured with an A/B process.
 
gammagore
#7 Posted : 6/24/2010 11:45:15 PM

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frinj wrote:
A more likely culprit is that, on the second (darkest) pull, I failed to rinse out my separatory funnel between the time I used it to separate the naptha from the MHRB solution, and the time I used it to separate the various washes from the naptha. I think this means that some MHRB residue could have been left on the inside of the funnel and could have through that way.

I plan to recrystalize all but the lightest 2-3 piles with heptane.


Thats sounds about right.

Your pics arent very clear but even on the second pic, from the left looks to have some contams in it. Re-x and a SC wash wont do any harmSmile

Be more carefull and more precise when separating and your spice will turn out much cleaner.

Happy extractions!!
 
 
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