What determines the length of time taken for the solvent and mix to separate?

[brainforest]

Hi

I am talking specifically about Cyb's salt tek here.

Can anyone tell me what/which factors determine how long it takes for the solvent and mixture to separate after shaking?

For example, I did the tek yesterday and they were separating in a matter of minutes after shaking. Today, using the same mixture and added lighter fluid it is taking about 30 - 40 mins. I am assuming that this is because the bark has had more time to break down and the mixture is therefore thicker and more concentrated. I've done this Tek hundreds of times but I'm just curious.

Thanks

Brainforest

 

[Tony6Strings]

I know you've done this a hundred times, but...

I usually wont shake a STB/boil'n'base because of the chance of emulsion. A properly basified acetic bark soup from A/B can be shaken up pretty safely without too much trouble separating. I love the glitter effect of the two layers separating back.

 

[brainforest]

HAHA

Thanks for the response, so if you don't shake what do you do? Just swirl?

Many thanks

Brainforest

 

[Tony6Strings]

I call it "rolling" the solvent. Turn your bottle 90° so the solution is along one side of the bottle or flask. Then turn your flask like a doorknob. Over and over in the same direction. One hand holds the flask, the other turns it.

 

[Jees]

For better separation: "More base" works if there was too little in it.

I've ran more than once in the situation where the more-base mantra did not resolve the emulsion. In those cases what did work was: more water (but make sure there is base enough).

The watery phase must be kind of watery enough. I had soups that were so much concentrated that I had to water them down again, only to discover a lightening fast separation after that.

If you notice a good separation in the first pull and lesser en lesser good separations the more pulls were done, I'd suggest to add water. Again make sure there's base enough because too less base is a ticket for a bad separation by fact.

I don't shake or roll any more as these methods need a closed recipient.
A glass jar with a loose lid on contains the black soup;
In microwave or bain-marie to make the soup hand warm, say 40 deg C (100degF);
Poor in solvent and stir the solvent in the soup with a glass or metal spoon;
Let separate, decant jar into a separation funnel or use a turkey baster to skim off.

This method makes a warm soup possible + solvent without the need for a closed recipient, I hate pressure build up in a closed recipient that I'm manipulating. One needs a very well ventilated place and some kind of spray paint mouth mask (carbon cartridge) because the recipient is open during the stirring. The advantage of a luke warm soup for better yields have been reported.

Happy trials.

 

[Tony6Strings]

Funny you should mention, jees, about closed containers building pressure making you nervous. A few days ago I had an acrb extraction in Erlenmeyer flask in a hot water bath on the stove. Usually I heat solvent and soup separately, this time I had them together from the beginning. Anyways, out of nowhere, the rubber stopper which had been placed firmly in the flask popped out with quite a bit of force. I didn't think much of it. Well, a few minutes later I had recapped my flask and was proceeding to roll my heated extraction. In the middle of rolling the flaskhow I described earlier in this thread, the rubber stopper once again shot out of the flask. This time it shot basified soup on my kitchen/living room floor, because it was on its side. I hurriedly grabbed the vinegar to neutralize a couple of spots which had gotten on myself and my girlfriend. After this I pulled the solvent while it was still hot, then cleaned up. It was crazy. Makes me nervous about using flask with rubber stopper. Its supposed to be safe. Usually it works just fine, this was just crazy.

 

[Jees]

Thanks for sharing that T6S, we can all learn from each other, especially the unfortunate things. Warmed products are safest not closed at all. If one wants to shake or roll then not warmed is a good idea. Then still, lids and stops can flip off, or letting things fall on the ground accidentally.

With my method the vessel is always safe and sound on a firm surface, no joggling. I've no magnetic stirrer, that would be cool, especially because the vessel can have that loose lid on always. For now I stir with a spoon, works absolutely like a charm but I have to deal with an open vessel so must ventilate very well and use that spray paint mask.

A magnetic stirrer hotplate is the best I guess.

 

[null24]

OK, wit cyb's and seperation issues, I've had sucess adding more saline solution.:?:

Probably not at the top of best safe practices, but putting the lid on a mason upside down, and laying out a bunch of towels on the floor, pref a garage floor or the like, and vigourusly rolling the jar back and forth, releasing pressure every few back and forths is a low tek barely safe thing I might have done to mix up warmish soup/nps mix.:?

 

[Tony6Strings]

I think I'm done rolling heated pulls in Erlenmeyer with rubber stopper. Think I may go back to a screw on lid for anything heated.

 

[Brennendes Wasser]

If the soup is not well filtered, then it may also take ages. Any fine particles left over will cause a time increase. But you can get rid of them by letting your soup sit for 10 h - may sound annoying to wait another time, but I would always do it, then you can easily decant, because all fine particles will have formed a solid sediment, that doesnt disturb when decanting any liquid :thumb_up: Maybe also more will form after you did a reduction step.

 

[Jees]

...I've had sucess adding more saline solution...

Hi null24, if what you added was salt dissolved in water, that water content in it's own right does water down the soup, which is something that worked for me as stated. The salt content does it own thing probably too.

Brennendes Wasser: I also like to filter my soups before reducing volume :thumb_up:

 

[null24]

if what you added was salt dissolved in water

Yeah, that. I threw my contact lenses away after eye surgery.

 

[merkin]

In the middle of rolling the flask how I described earlier in this thread, the rubber stopper once again shot out of the flask.

Haha. I do this way too often. I use a modified kjeldahl flask with a flattened bottom for extraction (nice long thin neck) and always seem to forget this is going to happen when the soup is around 40°. Keep reminding myself to vent first and make sure the stopper is secured well by my grip but somehow I usually waste a spurt at least once in an extraction. The pressure always catches me. Never seem to get the lesson.

Think I may go back to a screw on lid for anything heated.

Yup, I need to go back to the glass dude and get him to add a GL32 screw top to the flasks. He did that to an Erlenmeyer flask for me once.

 

[Northerner]

I used to use a large wine flagon with a cork, keep it in the sink with hot water to maintain temp. Tip it slowly upside down then back, release the pressure and then do it again until the gas releasing stage is over. Although not spraying basic solution everywhere if does tend to get a little basic solution around the top of the bottle so I'd use thick rubber gloves then once it was stable wash the whole thing off under the tap. Could put the gloves aside then for the rest of the process.

Got a stir plate now. Someone decided I needed one and gifted it to me.

As an experiment I've shaken solutions before. With some it's been fine and sorts itself out in 10 minutes or so but with a particular one the mess sat for days and required reheating and fiddling with to get the layers to separate. Even then more came out over the following days. I never bothered trying it again. Seemed like I was unnecessarily making the process difficult.