Y U NO SEPARATE?!?!

[Thre365ive]

Doing a STB extraction from Mimosa. Same way as I always do, but for some reason I added salt this time. Figured it couldn't hurt and that it might speed up separation.

Started with about 1/3 gallon of distilled water
Added 454g NaOH
Waited about 30 minutes
Added 500g mimosa powder
Waited about an hour
Added 300ml naptha
Turned end over end until mixed. No emulsion formed
Solution started to separate
Mixed again in the same manner
Added a few tbsp of salt
Mixed again in the same manner
No separation after 1.5 hours, so I added a bit more water, probably another 300ml per jug
Put jugs in a hot water bath, where they currently are now.

I usually use the heat from the NaOH instead of a heat bath, and I just make sure to do everything quickly. I always get separation within 10-15 minutes. This time I just have one layer.

Any ideas on how to get this separated and/or how it happened to begin with? I can't buy any more lye, because I bought the store out, lol. All I have on hand is household stuff, muriatic acid and solvents.

Update: after about 6 hours, it has finally started to separate. I added 300 ml of solvent and some more water (the jug is almost full of liquid now) and let it stay in the hot water bath. I've been changing the water about every 30 minutes, using mostly boiling water and a little cold tap water from the sink so it's not hot enough to melt the jugs.

 

[Thre365ive]

No ideas? This shit has been sitting since 4PM or so (it's now after 2AM) and it's still barely separated. I just do not understand the problem here. I've never had this much trouble with separation. Even if I get an emulsion, I can always just add salt and/or give it a heat bath and that breaks it instantly, but I don't get why the layers just aren't coming out.

I did use iodized salt, could this be the problem? I've used it before with no ill effects.

 

[Thre365ive]

I was thinking that worst-case scenario, I could acidify and just run an A/B on it. Would be a PITA, but it'd be better than not getting anything at all.

 

[cyb]

Salt is not the problem...in fact you can use the same amount as lye if you need to.
You have a hell of a lot of bark for that run...
What is the consistency of the mix?
It should be free flowing and not to sludgey...
You don't want to heat it up too much...it will pull lots of yellow..
If you used the exothermic reaction of lye to heat it in the beginning...that may have an adverse effect.

Make sure it is watery enough
And pull as soon as you get a stable layer..

 

[Thre365ive]

It's plenty watery, especially after adding more water. This is far from my first time, and I've made the mistake of making it too sludgy before.

I'm only using so much heat because nothing else seems to be working. The high heat is at least doing something. I expect it to be pretty yellow, but whatever. I can always recrystallize/ do a Clemmensen reduction on the leftover oils. I have plenty of naptha and a couple cans of n-heptane.

Really, I don't see how the salt (or more the iodine in the salt) could NOT be the problem. It doesn't make sense to me, but it was separating just fine before I added the salt. But as I said, I've done it exactly this way before with no problems.

I don't think the heat from the NaOH is the problem either. I always do it the same way and this is the first time this has happened. I let it cool to the point that I can pick the jug up for a good, long while before I add the bark. By the time I add the solvent, it's about as hot as a water bath would get it. It does come out yellow, but nothing that a recrystallization won't take care of.

If I'm wrong on any of these points, please let me know, but tell me why so I can make sure to not do that again, lol.

 

[cyb]

Re: Salt

The salt will have no effect on the ph as it is neutral in water solution..
It's only advantage is to raise the ionic strength of the solution and push more 'clumps' of molecule over to the non polar layer.

I must admit that all sounds fine with your extraction so am just as stumped as you..
Although have never used so much bark before so can't comment on your ratios..

Let's see what the rest of the world thinks when they wake up. (time zones are a bitch):d

 

[Thre365ive]

Re: Salt

The salt will have no effect on the ph as it is neutral in water solution..
It's only advantage is to raise the ionic strength of the solution and push more 'clumps' of molecule over to the non polar layer.

Yep, which is exactly why I added it. But I'm worried that I may have fucked up by using iodized salt. Thinking maybe I should have went with the non-iodized stuff.

I must admit that all sounds fine with your extraction so am just as stumped as you..
Although have never used so much bark before so can't comment on your ratios..

From my experience, my ratios should be fine. When working with a lb, you've got a little bit of play, since 10-20ml out of a 1.5L solution isn't gonna make much difference. Makes eyeballing possible, which is what I do. I've actually got a good bit more water in it now than what I usually use. I usually use 1/3 to 1/2 gallon of water.

Let's see what the rest of the world thinks when they wake up. (time zones are a bitch):d

Aren't they? Hopefully it all separates by then and this issue is null and void.

 

[Thre365ive]

So I got advice from another forum to throw it in the fridge. I did, and it kind of separated, but the top layer is still ridiculously dark. I'm gonna try a sodium carbonate wash and see what that does.

Anybody else got any advice? It's kinda hard to believe that nobody here has dealt with this before, and the search engine isn't turning up much.

 

[a1pha]

Did you check the FAQ?

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

 

[Thre365ive]

Yeah. I've tried everything up to the sodium carbonate wash and the extra ectraction. Cooking some baking soda now to make NaCO3. If that doesn't work, I'll try the extra A/B I guess. The only problem with that is that I can't get any more NaOH till the store restocks and I don't have a pH meter.

 

[Thre365ive]

I got it to mostly separate by putting it in the fridge. The solvent was still a pretty dark red, though. I gave it 4 sodium carbonate washes and it helped a lot, but it was still reddish orange. I threw what solvent I collected in the freezer to see what might fall out. I figure worst-case scenario, I have to re-x whatever's there. I have a couple cans of heptane and most of a gallon of naptha, so that's not a problem.

I think I'm gonna wait till after the weekend and get a pH meter to titrate the aqueous solution to pH 3 and just go with an A/B from there. It's gonna suck, but IDK how else to save it at this point and I have the HCl already. At least it should be defatted really, really well, lol.

I'm still open to ideas though.