So I was trying to follow the LLE wash procedure set forth in breaking dabs “cause i can” post which comprises of
5x LLE washes at PH4/5
1x at PH 8.4
5x more at PH4/5
PH 8.4 wash until pink no longer present in drained brine
1x PH4/5 w/ water completely drained
1x PH4/5 wash
1x PH neutral wash…
the issue im having is during the alkaline washes i am getting these crazy little beads of emulsion that fall to the bottom of the sep funnel. After the multiple washes leading up to the magsil collumn, only 20% of starting heptane solution remained leaving me to wonder where the rest went. I believe that non dissolved sodium bicarbonate in the saturated sodium bicarbonate brine solution may have interacted somehow with the resin…is this something anyone else has come across before?? worth noting my high PH brine only hit 7.6PH on a freshly calibrated digital probe, waiting on papers to check against since heptane washes can be hard to get a digital read on ive heard.
If this isnt the reason my possible reasons for 80% loss of solution are the following:
not waiting long enough for seperation
improper high ph value
reaction with solid sodium bicarbonate particles
lack of thourough agitation - (kitchen homoginizer for 3min bursts as opposed to reactor 10min mix)
RO instead of distilled water
taking breaks between washes for sleep/scheduled work
if anyone has some insight to what i may be seeing that would be great.
as of now the plan is to try and re wash with the spent water with longer wait times for seperation (possibly with a vibratory aid from local adult toy store)
to try and reclaim the lost resin and then start from scratch with what is collected.
pictures posted in following comments
Are you sure your brine is saturated? What is the water/ lab temp?
@anon42519203 any imput?
Lab temp is around 24c 75f…no more sodium bicarbonate would dissolve, granted I was hand stirring it for minutes at a time…
Or do you mean salt saturated? I did the 1lb/1gal salt to RO ratio.
Worth noting, adding heptane to the jar dissolved the beads and left just a white powder residue at the bottom (presumably the non dissolved sodium bicarbonate)
At this point I’m just doing what I can to get back all the resin possible and try to get back to a base starting point
What’s the amount of heptane and amount of distillate you started with? The water should be below the distillate layer but it looks like it’s on top here
Is it possible you used pentane and it evaporated? Or maybe an alcohol and it mixed with the water
You do not need to make saturated brine. There’s no evidence I’m aware of that brine works better than just using enough salt to prevent an emulsion. Brine should work worse than a 1% saline solution in my opinion
Did you make your brine with hot water?
Granted I have not read the OG Breaking Dabs post, but brine is typically NaCl saturated in water and not NaHCO3 - though I may be interpreting your response incorrectly. Either way, it takes about 1360g of NaCl to saturate one gallon of water.
Respectfully disagree. The saturated salt brine denatures existing lipo-proteins and allows them to partition into the aqueous fraction, for removal.
Brine pulls any water that the heptane holds onto back to the water layer
It’s .01% but not 0
Do you have experimental data that shows this happening? Something like recovered lipoproteins with brine vs without?
We’re talking first pass distillate, if there’s a meaningful amount of lipoproteins I’d love to test for them
That mignt have an effect on this processing. The magsil should catch that extra water. It might mess with the top layer of your mag sil.
Started as a 1:1 heptane:distillate…no pentane involved in process and ethanol should be moot do to distillation…
Did not mix brine hot, but 1lb of salt per gal dissolved with ease hand mixing to a crystal clear solution…would prefer to use homogenized or reactor, but the former overheats when used excessively and the latter is a couple paychecks away still
All the water used in these lle are brine I. The sense that 1lb NaCl was dissolved I to 1gal H2O…the “high Ph” fraction of these brine washes was achieved by saturating a volume of brine with NaHCO3 …
So 1lb /gal doesn’t quite fully saturate…brine may be a misnomer on this case my appologies
Heptanes water pulling capacity was one of the factors that keeps me coming back to that solvent system for lle…really want to explore/research other polar/nonpolar combos in time
This was what I thought as well. NaCl is safe, cheap, and loves water. CaCl2 is common for “drying” organic solvents too. I know the salt is dissolved in the brine solution, but it still pulls moisture into the sphere of hydration.
Here is what I found googling CaCl2 drying agent:
Test test… is this mic on??
That looks great @koilammmp super clean separation
Edit I do still see a few emulsion bubbles up top and about but the next rinse should break those, no? Maybe add a touch more heptane too?