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Need help revising my procedure for higher yields Options
 
Maxx
#1 Posted : 12/9/2013 12:27:30 AM

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Here's my basic STB procedure. I'm getting around .5-1%(usually <.7%) per extraction. Is there anything I can do to increase my yields?


Procedure:
Pour 100g MHRB into 1/2 gallon HDPE2 jug.
Mix 1500ml of distilled water with 85g NaOH in separate glass container
Pour the solution into the jug with the bark after the solution has cooled
Shake the jug until thoroughly mixed
Let the MHRB + lye water sit for a 24 hours.
After 24 hours, proceed with the first pull. Add 100ml Naphtha. Turn the container on different sides every few hours.
Retrieve Naphtha with mohr pipette after 24 hours and transfer to a glass jar
Repeat for 2 additional 24 hour pulls.
Transfer Naphtha to glass dish and place plastic wrap over the dish.
Freeze Naphtha until DMT has precipitated.
Carefully pour out Naphtha and retrieve finished product.

Suggestions? Mistakes in the process?

Note: I used 85g NaOH because in a previous extraction when I used 100g, the MHRB+lye solution ended up being very gloopy and when I did my naphtha pulls, the naphtha came out brownish, which then precipitated into a reddish brown gloop. Not sure if NaOH was the culprit and i'm open to explanations.
 

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dreamer042
#2 Posted : 12/9/2013 1:00:32 AM

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It sounds to me like you could be mixing the aqueous lye/bark/water solution with the solvent better. You need to be careful not to get too crazy and cause emulsions but you want to thoroughly mix the solvent through the aqueous solution.

Also the 24 waits are not really necessary, you can add the solvent immediately after basing and you typically want to mix the solvent through the aqueous solution and let it separate 3-4 times per pull, there is no need to wait hours between mixing, just long enough to let the layers separate again. After the 3-4 mixings you can go ahead and pull your solvent off and start the next pull.
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dooby
#3 Posted : 12/9/2013 1:09:53 AM

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What dreamer said, and maybe try adding 70 gr of NaCl (table salt) along with your base - it will increase the polarity of your base mix, thus "forcing" more alkaloids into your non polar solvent...
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Maxx
#4 Posted : 12/10/2013 9:23:02 PM

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dreamer042 wrote:
It sounds to me like you could be mixing the aqueous lye/bark/water solution with the solvent better. You need to be careful not to get too crazy and cause emulsions but you want to thoroughly mix the solvent through the aqueous solution.

Also the 24 waits are not really necessary, you can add the solvent immediately after basing and you typically want to mix the solvent through the aqueous solution and let it separate 3-4 times per pull, there is no need to wait hours between mixing, just long enough to let the layers separate again. After the 3-4 mixings you can go ahead and pull your solvent off and start the next pull.


By mixing better, do you mean mix along the lines of shaking the solution or stirring it?

 
dooby
#5 Posted : 12/10/2013 9:29:14 PM

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Stirring will not be adequate...

People do shake or roll their containers, or turn them end over end...

I pour and/or funnel...

As it's an STB process and I'm not familiar with those, you might want to follow dreamers advice and be careful not to create any emulsions though...

And salt Pleased
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