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Reducing Emulsion With Vacuum Pump Options
 
Shiva13
#1 Posted : 2/23/2016 11:36:30 PM

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After gently mixing my initial naphtha pull there was almost an inch of emulsion that did not seem to disappear after 20 minutes. I can be impatient at times so I decided to try a new way of getting rid of it. I have a harbor freight vacuum pump brake bleeder that I have been using to de-gas homemade wine and decided to attach it to the top of my extraction vessel.

After 18 inches Hg on the vessel, tinny bubbles began to raise from the basic soup and naphtha. As more bubbles were pulled the emulsion dropped considerably. It took about 5 minutes for the bubbles to stop. Every now and then I had to squeeze the trigger of the vacuum pump to get the vacuum back up.

Every subsequent mixing there was no emulsion at all and full separation was faster than I've ever seen. If I was to take a guess, I would say much of the initial emulsion problem was due to air trapped in the basic soup that developed during the initial steps of the extraction.

Here is the pump I used: http://www.harborfreight...c-vacuum-pump-39522.html
 

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BringsUsTogether
#2 Posted : 2/24/2016 2:10:25 AM

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Interesting find. I don't think I'll be using it, since I don't usually experience many emulsions with ACRB, but I'm sure someone might find it useful.
 
Shiva13
#3 Posted : 2/24/2016 2:36:43 AM

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generally I don't have issues with emulsion either. In this case I was not paying as much attention as usual. In both my salt and base steps I poured more aggressively than usual. This caused a lot of foaming and I'm assuming, entraining more air into the solution that made the emulsion more prone to forming. The pump pulled out a lot of that entrained air.

In the future I may continue to use the vacuum pump after adding my first naphtha pull if only to help speed up separation.
 
SnozzleBerry
#4 Posted : 2/24/2016 3:37:28 AM

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Up the base, no need for vacuums Smile

I used to base my solution to the point where I could shake vigorously and the phases would separate in under 30 seconds. This is one of several advantages that come with a/b over any method that leaves plant matter in solution.
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BringsUsTogether
#5 Posted : 2/24/2016 10:48:09 PM

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SnozzleBerry wrote:
Up the base, no need for vacuums Smile

I used to base my solution to the point where I could shake vigorously and the phases would separate in under 30 seconds. This is one of several advantages that come with a/b over any method that leaves plant matter in solution.


I use a tek that leaves plant matter in solution, but I just add about 70g lye and shake vigorously anyway. Haven't experienced much emulsion, and if I do, I just stir.
 
pitubo
#6 Posted : 2/24/2016 11:18:07 PM

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Like others already said, adding more NaOH will break emulsions. NaCl, and in general everything that increases the ionic strength of the polar phase, also helps to beat emulsions.

Be careful about pulling a vacuum on glassware. Only use undamaged laboratory glassware that is designed to withstand a vacuum. General purpose glass containers such as wine bottles and jugs could implode.
 
 
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