problem with acrb extraction

[lilayZee]

Hey,

This is only my second time attempting an extraction. Used Cybs tek to a tee with 50g of acrb. Everything was going great and looking on track until I added the naphtha (I used shellite as its the australian alternative). I got 2 shakes in with the resettling off the layers done in heat to help with the pulling and the layer at top was clear and it looked good. After my third shake up I noticed that the top layer wasn't clear, it was just really murky and it looked like it had solids floating around in there. I didn't really know if its an emulsion or not because I didn't see any bubbles. I let it settle for 24 hours and it just got thicker and the solids looked larger and more clumped up. I read somewhere that using a vibrator is a great trick for breaking up emulsions so I tried that and to no luck, looks like its going through the same process, but this time there is a very thin layer of bubbles in between the shellite and the rest. I snapped some photos of what it looks like after trying to use the vibrator and letting it settle for an hour. I read that dumping in more lye, and then more salt if it doesn't work can help out breaking emulsions. But didn't want to waste any resources not being sure if it was going to even help. Appreciate any help and advice.

 

[Ambivalent]

i dont know cybs tek, but slow separation usually happened to me if the soup asked for more base, or if it was too saturated with base or too viscous.

you said solids are floating in the nap. layer. this usually happened to me when the soup asked for more base, and plant fats more easily migrated in the upper layer. in this kind of situation adding 10 to 20 more g of base usually resolved the issue with separation and emulsion.

wish you luck. keep on reading

 

[lilayZee]

Yea I was thinking that the plant fats ended up in the shellite, just didn't know why or how.

Cheers for the tip.

Will be adding 25g of lye and i'll see what happens. Hopefully it will do the trick.

 

[lilayZee]

I added another 25 grams of lye straight into the mixture, gently rolled it and let it settle under heat twice. Still no good. The shellite layer is still murky and there is a big blob of something on top of the layer. I took these photos 2 hours after settling.

Anyone seen something like this before?

 

[Tryptallmine]

Last time I saw a layer like that was due to the fact that there was traces of detergent in my glassware.

Pull the naphtha from the glass and keep it aside, you can always back salt it to clean it up if there's anything in it. Suck up as much of that top layer as you can with a glass syringe or baster and put it in another glass/jar and set it aside. See if you can thin it out to a nice layer on your basic phase and try another pull with a fresh lot of naphtha. When you mix it through try not to shake it up or anything, just gently roll it end over end. Release any pressure as you find it building.

 

[lilayZee]

So I got around to adding some more salt and water together first as a last ditch effort to break the emulsion (if it is one). Same result, but after my first mix and settle under heat a lot of big bubbles appeared on the top and it took a couple hours to disappear by itself. I attached an image of this. So when i saw this I thought maybe the soap did contaminate the mixture because it looked like it was soap as it was bubbling. I don't see how it could have got in though as I'm pretty pedantic when it comes to these things, I use pretty much glassware for everything and wash it with soap and rinse it out really well and let it air dry till it is 100% dry, then I rinse with distilled water and let it dry 100% again.

I then sucked up as much of the top layer as I could and put it into another jar, still haven't got around to adding the new shellite. But now I'm thinking that it defiantly was an emulsion. In the other photo attached, that is about 75% of the the top layer that was murky that I sucked up sitting in a 100mL measuring cylinder, but I only added 50mL of shellite. It separated into three nice layers as you can see with the bottom one looking like it separated out as the base.

Does anyone know if this is an emulsion? Why has it only separated out again once I put it into the measuring cylinder?

 

[Tryptallmine]

When you clean your glassware - once its completely dry - wipe it out with 100% Acetone or Naphtha and let it evaporate.

If you do that as part of your cleaning ritual then you'll mitigate the issues with potential detergent contamination.

 

[lilayZee]

cool. thanks for the tip.

 

[BongWizard]

Tip for emulsion breaking: vibration. Most people sit the vessel on a subwoofer or a washing machine, but something I was told long ago which works almost as well as a fancy lab sonicator is to trim the tip of an electric vibrator (just a little one, we're not trying to make grandma squirt here lol) such that it fits snugly into the mouth of your separating vessel and crank it up. Goodbye nasty fat emulsions! 8)