Can't seem to pull anything, a bit baffled.

[MachineElf88]

Having a bit of a pickle, wonder if anyone can shed any light.

I did an a/b extraction with phosphoric acid on 380g MHRB. Split final liquid from acid boils in to 2 separate containers.

First container - added lye and pulled with solvent no problem and got a very pure end product, albeit a slightly low yield of about 1.3g

Second container - added lye and can't seem to pull anything.

I know its not the acidification that's the problem as my first container pulled fine. I have been struggling to get the PH high enough though. I've added 300g lye to 1 litre of solution in the 2nd container and can't seem to get the PH above 10. I was using PH paper to test.

I asked on this forum about the PH before I pulled and was told that the PH should be plenty high from the amount of lye I've added, probably over 14, so don't add any more. So I thought it was the paper just being hard to read properly as the liquid I'm testing is of a dark colour. Will get myself a digital PH meter in future.

I added solvent, mixed and pulled and got nothing. I then added more solvent mixed, left it over night, mixed some more and pulled and got nothing. I tried freezing and then evaping just to be sure but I kinda knew already it was empty as the solvent I pulled was totally clear, not milky or tinted in any way.

I'm a bit baffled as to what the problem is here. It's definitely not the acidification as I stated above. The only thing I can think is that the PH is just not high enough and I need to add more lye. Or I could add a lot more water and then add more lye?

Anyone have any ideas about what it could be?

Many thanks

 

[Vodsel]

Strange. There is obviously some difference between what's happening in both containers. Was the acidic extraction split after all the acidic cooks were mixed?

 

[MachineElf88]

Yes I collected all the acid cooks into 1 container and then poured half of it into another container.

 

[Vodsel]

If the base, solvent and container material are the same, and the pH is high enough, the only possible difference that comes to mind is the pulling temperature. Maybe you did a pull on the first container while the mix was still warm, and you tried the second at ambient temperature?

If so, you can try to give container 2 a nice safe hot water bath and pull again.

 

[MachineElf88]

Tried the warm water bath, still nothing. Well I say nothing but I did manage to get about 200mg from the last 2 pulls of translucent goo that then hardened into a yellow wax but that's nothing to write home about. Couldn't be more different from the pure product I got from the first container.

It must be the ph level. At lower ph's is it more likely to pull other gunk as well?

I think I'll have to add more water and lye.

 

[psychonut]

That is an incredible amount of NaOH, I feel sure your pH is PLENTY high. Try splitting up your liquid into 250 ml portions before you add water, that way if something works you can apply to the rest and if it doesn't you aren't completely screwed. Try adding 50 ml H2O to 250ml of solution and 75ml to another 250 and so on.
Also, agitation and contact btwn solution and solvent is more important than heat. Yes, more heat will allow a more saturated solution, however; you aren't pulling anything.
Try a mixer on slow speed w/only one beater attached, this will mix it w/o to much emulsion.
Oh, you are more likely to pull "other gunk" with to high a pH than too low.