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A fix for emulsion(?) Seemed to work for SWIM!

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DimensionlessBeing

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Swim had emulsion in a lye/Naptha extraction. With little patience he took the turkey baster and sucked the emulsion up and instead of discarding it, he stuck the emulsion filled turkey baster deep into the mhrb/water/lye mix and squeezed the bulb very slowly until it was emptied. Naptha rose to the top and mhrb/lye/whatever that made up the emulsion was gone. swims turkey baster has an injection needle on the end of it. The needle has been ground flat and crimped into a slit because swim found that the slanted head of the needle let air go in while transferring pulls to an empty jar. The tip was then crimped to a slit because swim found that the turkey baster pulled with too much power. Both fixes solved problems with the turkey baster and may have helped with breaking the emulsion when swim sucked/injected it.

Hope this info helps someone...
 
Nice "lab" notes and thanks for sharing, these do come very handy time to time, your lab books are priceless. You can always prevent it happening in the first place by gentle end over end turning with some patients :)
 
Nice tip mate :)
Until now I've always just added lye and then my emulsions have always gone. But this tip can save me lye, which is a good thing because lye can be hard to find where I live.

Thanx for sharing. Will try this next time.
 
swim has used this method twice now. On the last batch he started shaking instead of gentle rolling the jar to intentionally create emulsion. He wasnt dissapointed. Emulsion formed, he got is turkey baster and hot water bath ready. Two hrs later crystal clear yellow pull with 300mg yield on the 3rd pull!
 
What do you mean by suck up the emulsion? My MHRB/water/lye mixes are always black so you can't see into them, do you mean you just slowly suck up some of the mix and then slowly squeeze it back out?
 
DimensionlessBeing said:
With little patience he took the turkey baster and sucked the emulsion up and instead of discarding it, he stuck the emulsion filled turkey baster deep into the mhrb/water/lye mix and squeezed the bulb very slowly until it was emptied. Naptha rose to the top...

I'm referring to this part where he said he sucked up the emulsion. I might be wrong but doesn't an emulsion here mean that there's naptha in the mix that's not at the top? I'm just wondering how he sucked up the emulsion since I can't see into my mix and I assume he can't either.
 
after shaking the mhrb/lye/water/naptha, if there is an emulsion formed of the naptha and the other ingredients, that emulsion is what i was referring to. the emulsion in the instances spoken about in my post, resulted in the naptha layer being 50% emulsion, 50% clear naptha. It was a layer between the un-emulsified naptha and the m/l/w mix. it looked like bubbles and would not settle out.
 
btw, I'd be interested in feedback on anyone who tries this. while i have replicated it now, It would be encouraging to hear that it works for others. Then it could be added as a sticky to make it easy to spot for others.
 
@L_Starr, I assume then that you're using a separatory for this step? Or just inverting it in a bottle?

Also, @dimensionless, if you know the syringe isn't air-tight, boxes of Pasteur pipettes and some bulbs are easily available (or a few pumps and a set of Mohr pipettes) and might save some time and effort. I'm concerned that eventually that tip is going to get clogged or even worse break off into your separation vessel from being stressed, or, as you said, you're going to have to repeat extractions because of unpredictable flow. With glass pipettes, it also seems easier to recover anything left after pickup by removing the suction device and rinsing through with solvent. If it works, though, it works :); those pipettes are easily *found*, but you'll also have to drop some good dime on them and hope you don't break too many/any of the Mohrs. :) I will definitely keep the syringe tip in mind, though, if I get to it and find that I'm totally wrong about the pipettes handling emulsified stuff better.

If one were apprehensive about pulling up a bubbly layer period, do you think your mixture would've settled out if you'd removed the majority of the liquid naphtha and inverted/shook it again with the tiny fraction?
 
Ansar said:
What do you mean by suck up the emulsion? My MHRB/water/lye mixes are always black so you can't see into them, do you mean you just slowly suck up some of the mix and then slowly squeeze it back out?

If you get an emulsion it will form in between the black bottom layer and the top layer of Naphtha. It will look like a layer of bubbles seperating the layers.

If it's just 2 layers, 1 black at the bottom and then your solvent on top you're good. It's not hard to spot, you'll know it when you see it.

Hope this helps :)

Peace.
 
AllIDoIsSWIM said:
If one were apprehensive about pulling up a bubbly layer period, do you think your mixture would've settled out if you'd removed the majority of the liquid naphtha and inverted/shook it again with the tiny fraction?


No idea. not much experience with emulsion. The two times I got it I used the procedure I posted.
 
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