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Something has gone awry in my AB extraction Options
 
Shambolic
#1 Posted : 6/27/2014 10:49:34 AM

I am down with the funky shit


Posts: 7
Joined: 14-Jun-2014
Last visit: 22-Jul-2014
I was wondering if anyone might be able to shed light on my issue....? I would post in main extraction forum, but can't due to restrictions on new members.

I've run through a typical AB extraction of 1kg of MHRB. Boiled in acetic acid @ approx pH 3.
Reduced to a few litres and allowed to cool, filtered and separated from sludge.

Then basified with 50g of NaOH to pH 12 plus (pH meter struggled with extreme pH)

This was left for a week while I worked on some ACRB.

I only had 400 mL of naptha (waiting for order), so I seperated approximately 1.5 L and heated in a bath with 100 mL of naptha. This was mixed and then allowed to settle and layers form. It looked fine, no emulsion. This was repeated with another 100 mL, and then 200 mL.

As soon as it cooled to room temp it was good and cloudy. There was a few blobs of base in the jar which I separated out when I put naptha in a dish for freeze precip.

Now this is where I notice something isn't right. It smells of NaOH or caustic soda (lye in american) Neutral

After a night in the freezer I can see normal looking crystals formed on the glass and atop a layer of creamy sludge which I assume to be NaOH that has somehow got into the naptha layer. There was definatly no base solution in the dish after seperation. The creamy sludge was already in the naptha after seperation from the base layer.

What has caused this to occur? Have I over basified my initial base? Was it too hot? Did I not leave it long enough to seperate out (unlikely as it had separated perfectly) ? Was there not enough naptha in ratio to base solution? I just assumed from my chemistry knowledge that the naptha would simply take on as much DMT as it could before reaching saturation point, then I can do further pulls when I have more naptha....

And how do I recover the DMT from the naptha now? I'm thinking of doing an acid wash to but unsure if it will work if there's NaOH in the naptha?

Any thoughts or comments would greatly appreciated
Didadamdooooo.... Yeah yeah yeah but nah nah nah
 

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--Shadow
#2 Posted : 6/27/2014 12:59:24 PM

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Joined: 21-Dec-2013
Last visit: 28-Dec-2019
Now I'm not too sure with MHRB specifically, but with acacia material what can happen when you leave the soup basified too long, gums and oils tend to come across more into your naptha.

From here, I would suggest doing a mini-AB on it or wash with some H2O (shouldn't need any NaOH as the DMT and solution is in a basic state already)

Then a re-X to be sure.



Throughout recorded time and long before, trees have stood as sentinels, wise yet silent, patiently accumulating their rings while the storms of history have raged around them --The living wisdom of trees, Fred Hageneder
 
 
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