is the spice in my emulsion?

[smc123]

2 kilos mhrb soaked and filtered with ~6.5 gallons of acetic acid solution over the course of ~18 hours.

Extract was collected in a 7.5 gallon bottle and basified to 12.5 with sodium hydroxide.

Multpile pulls of naphtha, freeze precipitated, yielded 5 even grams of spice.


Could the 1 inch emulsion layer yield more spice? Was some possibly missed?

 

[d*l*b]

I would hope that there would be 15–30g to be pulled from 2kg, so i guess there should be more to be retrieved. How much solvent are you pulling with?

Have you tried anything to get your emulsion settled? Lots of info here: Emulsions From Hell

 

[smc123]

The initial pull was about a quart with half removed to freeze precipitate and the replaced by fresh solvent.

On the third extraction as much solvent as possible was removed.

Extraction totals: 1st - 3.2 2nd - 1.4 3rd - > .5


The emulsion hasn't been touched. I'm checkin that link now.

 

[smc123]

The emulsion as well as a small portion of the basified solution (still pH 12.5) was removed and placed in a seperate jar.

To the jar was added 125 grams of NaOH and 1 cup of water, and the mixture was shaken, vigorously.

The result was almost complete seperation of the emulsion. This also yielded .9g on first pull.


To answer the question, it seems an emulsion does contain spice.

 

[bongz]

your yields still seem extraordinarily low, You may want to increase the amount of sodium hydroxide added to your bark solution and do more pulls, perhaps agitating for longer when the naptha is in contact with the solution or even doing heated naptha pulls. swim told me it would probably increase your yields.

 

[smc123]

Another pull was done, after adding ~150g NaOH, with ~a pint of solvent. The basified solution w/ solvent was agitated for 15 minutes, and after freeze precipitation yielded 1.5g.

Thanks Bongz

Current combined yield: 7.8g

 

[smc123]

6 additional pulls resulted in excellent crystal formation but after collection and drying yielded 5.2g of yellow oil.

~1 pint of warm naphta was added to the oil, mixed gently, left to evaporate to half original volume. The solvent was then decanted and the oil left settled at the bottom.

Freeze precipitation from this yielded 2.5g. No oil.

 

[smc123]

Final yield was 12.2g clean DMT from 1975g MHRB ( 0.618 % ).