OKAY. Not so much of a problem as it is a puzzle...

[athousandeyes]

Okay, yield is looking GREAT at 1.6%. (last pull was 4.05 overall out of 250g MHRB) BUUUUT seems to be grabbing the last almost ENTIRE solvent pull. Using heat, both exothermic in the beginning after it drops below 120 degrees F., then a hot water bath in the tub (peaks at 117.8 degrees F., brings aqueous mixture's temp to ~105 F.), also, trying not to aerate the solution with stirring texhnique, but it seems to form a pretty decent emulsion no matter how gentle one is. Which is weird, because 1:1:15 is supposed to give the proper pH of 13.5 where spice is fb'ed and emulsion supposedly "cannot form", right? Lab still lacks pH metering, to come soon. Anyway, yield is great, not a problem, but in the last few runs there has been a trend, after going over the documentation, of the first and last pull not crashing all the way out, but the second pull is coming out right on the nose, no extra. Where is the solvent going?! I know its right there! Why won't it fall out? And is another 50 ml of solvent going to increase yield in any kind of noticeable way?

 

[Enoon]

Sorry, I don't quite understand what you're saying...

1) you are getting emulsion?
or 2) your solvent seems to be disappearing?

Are you sure it's not just evaporating due to the heat you are adding? naphtha has a way of escaping even some closed lid containers IME... Emulsions can also sometimes form if there is too little water, but given your ratios that shouldn't be a problem.

maybe explain your issue a little more clearly and someone can help you
cheers
Enoon

 

[athousandeyes]

okay sorry, the tek used was a variation I came up with of vovin's A/B, but just STB, and the equipment isn't lab grade, by any means... The problem is that the solvent is disappearing, but only after the first and last of 3 pulls, either solvent, too. I know it isn't evaporating, because the way the math is worked out, when I pour the little jug into the big jug it goes up to the neck, and by the 3rd pentane pull and even more so by the 3rd toluol pull (6th) the whole liquid volume has increased to where, oh, 100-150 ml stay in the little jug. AND there is a dark pink, small bubbled emulsion resting underneath a burgundy, big bubbled emulsion, there are 2 clear layers. This is happening EVERY time, that is why it is notable. And again, yield numbers are good, but I'm thinking they could be better, and I'm wondering how much spice I have flushed down the toilet getting rid of base mixture.

 

[Noman]

First, 1:1:15 give a pH way beyond 13.5.
STB teks use an excess of lye to do the work of breaking down the plant material that happens in the acid cook of an A/B. It's only with A/Bs that 13.5 is the target pH, and that requires a fraction of the lye used in an STB.
So are you doing three pulls with pentane and then three with toluene?
I've never pulled with pentane, so I have no idea how it acts, but my thought is that on the first pull you're getting plant crud that is forming your emulsion which is mostly gone by the second, so you get a clean second pull. I've heard of later pulls forming emulsions, but never had it happen, so I don't know what's going on there. Maybe as the bark is given time to break down further, more plant crud is freed up?
Still doesn't explain why they would form on the first and third pulls with both kinds of solvent though.
The good news is that all you have to do is remove the bottom layer of clear aqueous solution and stir warm basified water into the emulsion. You might have to do this a couple of times, but that should break the solvent out. You might help things along by adding a little bit of clean solvent too, if it's just emulsion with no clear solvent on top.

 

[athousandeyes]

Cool! Very informative and helpful! Going to check on the second pull of a little experiment... 6 pulls toluol, 75 ml each, on pull 2 with some DARK yellow solvent. Much love, fellow nexian!

 

[athousandeyes]

Emulsions aren't forming due to an updated trick: adding more base after each pull. Works like a charm! Still in progress, results pending!

 

[athousandeyes]

Pending evaporation, monumental success! Pics, or no?

 

[Ljosalfar]

Sure, pics are always encouraging for the rest of us 8)
Not sure, but I believe you can freeze precip from the pentane - worth a shot. Toluene won't.
Best,
L

 

[athousandeyes]

6 pulls toluene (75 ml a pull) heated STB add lye (about 5-10g) every pull to re-base the solution, minimal loss from recovery, weird emulsions form when the solvent gets to a supersaturated state (smokin' ganj and bullshitting away for 45 minutes during a pull then heating it will do that) but nothing a few little pokes and prods and good ol' time don't solve. Ok all that out of the way, the result was a whopping 3.95 out of 250 grams of MHRB.

 

[Enoon]

That's a pretty good yield you got there, congrats.
and thanks for the update and your trick. maybe it helps others that run into the same problem.

cheers
Enoon

 

[athousandeyes]

did a "quick pull" where added 50 ml fresh solvent, busted emulsion formed, my speculation is that the solvent was over saturated with the molecule and the fats and the oils, so it couldn't separate. I am waiting on results from the last 250g batch, it looks more abundant than the 1.58% last time....

 

[athousandeyes]

literally identical yields two times on 250g MHRB. :d