Heating acid/base solution prior to addition of naphtha helps separation--any disadvantages?

[Emperor Norton]

Hello everyone, it's wonderful to see the site back up finally. I've been a lurker around here for quite a while now and finally decided to make an account since I feel like I'm at the point where I might have something to contribute occasionally.

So far it strikes me that the most difficult and time-consuming step in most extraction teks is using the separatory funnel. In my first couple of extractions, I always had a terrible time trying to get rid of the emulsions that seem to inevitably form between layers no matter how gently I stir them. I read on here that warm naphtha separates much faster, but heating it prior to addition only seemed to help a little bit. Finally I realized the problem was that the acid / base solution (depending on whether I was defatting or pulling) was immediately sapping all the heat out of the naphtha. When I heated the aqueous solution AND the naphtha, the naphtha stayed warm and separated much more easily!

Is there any reason most teks don't advise us to do this? Does heating the aqueous layer make DMT less prone to moving into the nonpolar layer, or something?

 

[t0kin]

It's been discussed a few times and the general consensus is that heat when pulling results in more transferred. That means more transfer of spice as well as other impurities. A little heat shouldn't cause any problems, but if your having trouble separating at room temperature it may be because of something else. Not enough water (#1) or lye (#2) are the big problems I've seen. Most of the separation should occur within 20-30 min tops if you have the right mhrb/water/lye ratio, but heat will speed it up. I haven't seen a single emulsion since using this ratio (15+ml:1g) with STB teks. What tek are you using?

 

[Emperor Norton]

Most recently I've been experimenting with a soxhlet, so I'm not really following any established tek anymore. You're right that most of the separation usually completed within 30 minutes, but I usually found myself left with a thin ring of very fine foam around the edge that showed no signs of dissipating even after several hours. Heating up the water prior to adding the warm naphtha has allowed me to get perfect separations in only a couple of minutes or so. None of this will be an issue for me anymore pretty soon, since I've ordered a CLLE, but I figured others might find the technique helpful if it doesn't have any downsides.