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whitebread420
#1 Posted : 7/24/2012 3:29:40 AM
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Posts: 58
Joined: 19-Oct-2011
Last visit: 14-Apr-2016
Location: US
hello all

first let me say thanks for all the help so far because I have come a long way with my extraction techniques and I successfully can get about a 1.6% yield.. way up from a 0.5% average before.

with 250 g MHRB powder, I did 3 acid cooks while stirring at a simmer for an hour each. I did this again with another 250g powder. This left me with 4L of acidic, dark red water. I added 250 g NaOH, and the solution of course turned very dark black.

while heating (below a simmer) I did my first naptha pull while stirring. emulsions don't form immediately, but it seems that while heating and after 10 minutes or so while stirring, an uber emulsion will form (i mean there's NO separation at ALL). I pull out where the separation line should be, put that in a smaller flask and add NaCl. This breaks the emulsion, but makes the naptha very reddish in color. Not a big deal .. just tedious.

pulls 2 and 3 are the same story. on pull 4 emulsions don't form anymore and the naptha looks the more normal yellow in color, and about 7 pulls in total are needed for the naptha to come up clear. each pull is allowed to stir for at least 20 minutes.

I did not evaporate, instead put the combined pulls in the freezer. Like i said .. i got a little over 8 grams after drying. about 1/3 of it looks like the pure-er white DMT, while the other 2/3 is a light brown. I mixed it all together and bio-assayed ... and it is very very potent. i would say much stronger than just the white DMT and i enjoy this a lot i would say

with the rest of the naptha i reduced to about 1/3 with use of heat and a fan and put it in the freezer. heres my question:

what i got was a whitish yellowish substance that wasn't quite hardened (and i'm wondering what it is) .. so i couldn't decant the naptha. I have it evaporating now at room temp as i feel this is my only choice and i will let you know what i get.

my second question, should the basified soup be warm ... not so much "hot". i feel this is the culprit to the emulsion formation. also ... it's what is making the naptha solution very reddish in color.

next time i'm going to defat before basifying .. i just read about this in another thread and wish i thought of it before... always learning, huh? lol

also i guess i need to try a calcium carbonate wash step .. which i'm not looking forward to because i've purchased sooooo many supplies already lol
 

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Dinosaurr
#2 Posted : 7/25/2012 2:14:14 PM
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Joined: 22-Nov-2009
Last visit: 23-Oct-2012
Location: Mars
How were you heating? In my experience, it is MUCH easier and efficent to heat the solvent for each wash instead of a hot water bath for the whole jar(which may also be a culprit). The red solvent layer is infamous, I think it has something to do with micro suspended rootbark in the solvent. Whatever it is, there is a simple fix. DO NOT evaporate the soloution fully yet, reconstitute with naptha and wash with a slightly basic soloution. Sodium carbonate (washing soda) would be the base of choice. Mix in a jar, even shake it a little bit, and let it separate and siphon off the solvent. One wash should be enough to rid most of it, what little left will be in the bottom of whatever container you put the solvent in. Pretty easy to pour off the solvent and leave the rest in the jar/measuring cup.

Baking soda is cheap, somewhere around here there is a tek for heating it in the oven to convert it to sodium carbonate. So that shouldn't stop you from the wash step.
 
 
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