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Help! Contamination from heated HDPE? Options
 
davedaviddavidson
#1 Posted : 7/7/2011 4:04:03 PM

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Hello, SWIM is performing his 3rd extraction from MHRB using Norman’s tek and has encountered a problem. His previous attempts have been very successful, the only differences this time are that a HDPE container is being used instead of glass, and the lye was dissolved in hot water, then the bark was dissolved and left to sit for 1 hour, then warm naphtha was added whilst the MHRB solution was still very warm.
The naphtha that was pulled after agitation was a non-translucent very dark brown/red color, SWIM was pleased to see a light precipitate forming as the warm naphtha came in contact with the cold glass dish he was decanting it into.
However after cooling down some clear jelly like substance was forming in blobs above the thick dark sludge at the bottom, after being placed in the freezer the clear jelly had now disappeared but the dark naphtha couldn’t be separated from the sludge at the bottom through filtering as it wouldn’t pass through the filter and any residue left in the filter was absorbed by the paper and couldn’t be scraped off.
SWIM is now attempting a recrystallization; he has re-dissolved the sludge in hot naphtha and has been left with a black solution which is now cooling, buy can already see the sludge reforming at the bottom of the glass. Has anyone ever encountered this problem before? Could it be that the heat caused a foreign chemical from the HDPE container to seep into the naphtha? Any advice would be very much appreciated. Thanks
 

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HermeticShaman
#2 Posted : 7/7/2011 5:21:57 PM

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There really shouldn't be a problem between naphtha and HDPE container. Ive had a similar problem with other plastics and xylene, but never naphtha. I wonder if the lye doesn't agree with the plastic. Perhaps someone else will know
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davedaviddavidson
#3 Posted : 7/7/2011 6:55:39 PM

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Yes I think you’re right, SWIM noticed that whilst adding the lye the additional heat given off cased the container to become softer than before. This seems like the most plausible cause of contamination which was then absorbed by the naphtha once it was released. SWIM is going to try a few recrystallizations in the hope that the spice can be separated from the sludge and dark naphtha but is stuck for ideas other than that.
 
mshanksman
#4 Posted : 7/7/2011 9:54:11 PM
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This concerns me because I used an HDPE container too, although, for me, the naphtha was never dark, tan, or brown, just cloudy / piss colored. I mixed my lye separately in a glass container, though, and didn't add it to the HDPE container until it was cool enough to touch. When I did my hot pull I used water that had been boiled and allowed to cool a bit, since I read that the safe prolonged exposure temperature for HDPE is about 100 degrees C, or, slightly under boiling temp at my altitude.

I bet if you do a re-x you should be fine..?
 
endlessness
#5 Posted : 7/7/2011 9:57:26 PM

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FAQ question 4.13: https://wiki.dmt-nexus.m...FDark.2C_what_to_do_.3F

I would guess thats your problem. In any case, if you would want to make 100% sure there is no phthalates or other plastic remains in your dmt, the best way to guarantee would be to salt out your dmt from solvent with, say, fumaric acid, and then do an acetone wash. But I would guess your issue is rather the one mentioned in FAQ.
 
Psyvox
#6 Posted : 7/7/2011 11:22:04 PM
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Why did you dissolve your lye in hot water? Sounds dangerous to me
I'm SWIM
 
davedaviddavidson
#7 Posted : 7/7/2011 11:59:21 PM

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Thank you all for your feedback Very happy
I will finish the recrystallization and if that fails I’ll try a sodium carbonate wash and see what happens.
 
davedaviddavidson
#8 Posted : 7/9/2011 4:27:19 PM

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I used heat because I wanted to keep the naphtha as warm as possible to encourage it to absorb the dmt in the solution.
I’m just doing a sodium carbonate wash on the very dark naphtha and after shaking vigorously only some of the now yellow naphtha has separated to the top, in-between the black water and the naphtha there is a thick layer of Bailys colored emulsion that won’t separate. I’ve never experienced this before and am not sure what to do about it.
 
Psyvox
#9 Posted : 7/9/2011 5:26:45 PM
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davedaviddavidson wrote:
I used heat because I wanted to keep the naphtha as warm as possible to encourage it to absorb the dmt in the solution.
I’m just doing a sodium carbonate wash on the very dark naphtha and after shaking vigorously only some of the now yellow naphtha has separated to the top, in-between the black water and the naphtha there is a thick layer of Bailys colored emulsion that won’t separate. I’ve never experienced this before and am not sure what to do about it.


Just be carefull. The hot water enhances the extreme exothermic reaction and can even make your water boil, making it more likely to spill. I suggest using water on room temperature and warming up your naphta with something else.
I'm SWIM
 
d*l*b
#10 Posted : 7/10/2011 12:27:49 AM

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Also to note that the hotter your solvent, the more impurities you will pull along with it. In the last extraction I did I added solvent moments after adding the NaOH and, while I pulled almost everything in one go there was a lot of gack to be that had to be removed by re-x after.

If I wish to do hot pulls I generally either add solvent while the solution is still warm (not hot like I was saying above) from adding the base or by keeping the container in a water bath.
D × V × F > R
 
benzyme
#11 Posted : 7/10/2011 12:40:14 AM

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HermeticShaman wrote:
There really shouldn't be a problem between naphtha and HDPE container. Ive had a similar problem with other plastics and xylene, but never naphtha. I wonder if the lye doesn't agree with the plastic. Perhaps someone else will know


lye doesn't affect the plastic, but naptha will if it contains aromatics.
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