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
Magsil collumn
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:
evaporation
transfer loss
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.
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
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.
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.
