Hoping someone can chime in with some brine wash tips.
1st run - diluted 3 to 1 heptane to crude. 5 total gallons. 5 grams citic per liter of solution for degum and mixed in. Then two 5 gallon buckets ph4. One ph neutral bucket then high ph bucket finished off with 2-3 neutral buckets. At the end of washes I ended up with half 2.5 gallons of crude/heptane.
Used big spoon to mix
Threw away all the emulsion/waste water out! (Don’t make this mistake)!
2nd run - dilute in 4 to 1 hep to crude. Citric acid swirl first. Started with two ph4 buckets that took me from 4 gallons hep/crude to 3 gallons. After did a neutral wash and the wash didn’t separate.
I kept the “waste water” of the two buckets and noticed hep floating on top. So I figured to mix the waste bucket and my neutral “emulsion” mix together in hope it would all separate. After a few hours it separated only leaving a tiny thin layer of hep at the top.
" Used a cake mixer to mix.
Is the cake mixer messing me up? Or should I just mix softer with a big spoon?
Can anyone help with why I’m loosing so much hep to the washes/emulsion?
Also is there any advice on how I could salvage or push the cannabinoids out of this big crazy mixture i have going ?
U shouldnt be losing that much, and im assuming ur losing most of it when ur dumping ur emolsion layer.
Catching the emulsion in a bucket is a good idea. And not sure why u werent able to recover most of ur lost heptane that way.
I do half the size batches u do and only lose maybe 500ml.
I mix vigorously for 10 min, let settle for 15 min and dump out the water layer. And collect the emulsion in a sep funnel, by the time the next run is done the sep funnel should have seperated most of it. Keep dumping into the sep funnel until its full. Put that in a bottle to run later with ur next batch. I wouldnt mix this portion back into the first batch ur trying to clean up, youll just go back 3 steps. But cleaning it on its own when u have extra time is the best solution to that nasty emulsion layer.
If u have some emulsions that are taking forever to break, add in 5-10% salt, mix then let it settle. Emulsion should break in a few minutes. Adding in salt to ur bucket might make some heptane percipitate out aswell.
Thanks for explaining. I’m confused to why my last neutral brine bucket didn’t even separate? Only difference was the paint mixer. Could this of mixes it so well it doesn’t want to separate? At this point, it’s all mixed together. Waste buckets and emulsion mix. There’s think layer hep on the top although I know there’s much more hep in the mix? There’s already 5% salt in it. You recommend add more salt and it will help heptane float to top?
First two buckets I waited 10 minutes and noticed hep at te too of waste after I separated. Then I waited 15 minutes on neutral bucket and it didn’t separate at all. Threw all the mixtures back together and after a night it only separated a very thin layer… thanks for you input!
In total washed will equate to 15-18 in total(not entirely as many needed if done right, I set for this many to ensure all unwanted are removed.), sets of 3,3,4,5 or 5,5,3,5. First washes high ph to 12ph with SB & probe till ph is adequate for wash & not a over saturated solution, wash vigorously for 15-20 minutes, then Let settle for up to 30 minutes+ & remove emulsion (but save to seperate the rest of heptane/ cannabanoids in second wash out). Then with low 3-3.5ph with citric to have A swing just in case to remediate any other soluble compounds not wanted with a schwinnnng for another 20-25 minutes & settle for 30 minutes discard emulsion to secondary bucket for another wash/ seperation later. Then brine to wash (5% saline solution water/salt) out any solubles/emulsion that may still be in the solution 15-25 minutes vigorously stirring then settle for 30 minutes+ (completely remove all gunked up emulsion before last wash). Then finally 5.5-7ph wash with distilled or DI water till ph mimics water going into washes after coming out (stir for 15-20 minutes, seperate for 30-40 minutes), & remove organic layer(s) (layers depending the size of their sep funnel or if their in the reactor it’s easier to do washes then seperate.) the bases for ph will be sodium bicarbonate & citric acid. Ph accordingly with a digital probe for best results in ph solution (papers are easier once you get dialed in on how much needed for each solution etc).
Keep in mind I adjusted the detail in washes for singular washes not for the multiple washes as described in the first lines. If doing multiple washes per set, prep accordingly for each step to streamline the process & ALWAYS BE THOROUGH.
Edit: pictures for reference of singular washes from a client( been cropped to only see colors etc).
From purple - removal of oxidative compounds - brine wash clarity etc - clear final wash
Try skipping the degum, I tried that tek according to Columbus labs sop or whatever that had similar amounts and I found small amounts of citric acid drop the pH sufficiently. I’m not sure an acid wash is even necessary tbh.
I understand the logic, I’m wondering how many people have compared with vs without. I don’t acid wash anymore, only if I know I am doing pest remediations will I include a light acid wash.
Also are people watching their pH go down or just throwing powders in water according to sops…
Big thanks for your detailed explanation. Is the only reason one would loose so much hep in the washes is because I’m not waiting long enough for it to separate?
Which sodium bicarbonate do you buy? The one from bvv was weak.
@anon45638961 I am using a probe to dial ph in. Thanks!
Now that i lost all my hep/product to emulsion layers and mixed it back together in one big batch. Is adding more salt the best way to push the hep out of the emulsion layer?
BVV is only good for stainless imo or some other equipment, they treat powders/ reagents if any like shit in my experience. Crap storage & shipping, I’ve had a bag show up ripped of T5 never ordered there again.
Use a supply store like smith scientific supply or a online store like sigma for better results.
Mix at high rpm for 20+ minutes make sure nothing is settling, then let seperate while on slow rpms, should do fine, only suggest to get you heptane/ water back to a 1:1 then do it.
thanks … which song do you suggest? ill try it out!
Figured out that the best way to break up the emulsion layer is to wash the layer itself vigorously with a 1 to 1 brine wash then let it sit for 12 hrs. After washing the emulsion layer twice i reclaimed all the hep/crude I thought I lost. Thanks community for your help! Hope this post helps ones in the future !
Also noticed that the more vigorous I stirred my washes the more emulsion showed up. Now I’m happy with a hand swirl instead of high rpm paint mixer.
today 
thanks … which song do you suggest? ill try it out!