Be sure to look at the newly updated version of this (11/2019)
It’s important to have a basic understanding of Advanced Short Path Distillation before diving into the advanced techniques. We suggest reading some of our previous articles on fractional distillation & engaging with some hands on experience to perfect operation of the equipment. This is information that we make openly available, while others may charge for consultations you can find a major resource here. This process was refined through benchmark testing with numerous skilled technicians.
Mastering Winterization – Fat, Lipid, Wax Removal Process
This process of winterization was originally developed by Summit Research during our early stages of R&D. We’ve changed things up to improve efficiency compared to traditional winterization techniques. Here is the original Summit Research winterization technique :
- Melt down your base starting material (oleoresin) at a 1:10 ratio with alcohol to create a “solution”.
- Place the solution in a deep freezer. If it’s dry ice ice 30-60 minutes / if it’s in a cryo freezer this may take 12-24 hours.
- Allow the solution to begin “waxing” up than remove from the freezer.
- Leave the solution out to warm up, keeping it at least 20 degrees below room temp. This allows major components to precipitate from the solution.
- Begin a large micron filtration, in our case we use a Hochstrom with a stage 1 (20 micron) chemical duty paper.
All filtration with hochstrom filter only need to be at half vacuum for full flow.
The pass of semi-cold fluids will now flow with improved efficiency. You will “rough cut” the solution & remove a major part of the mass, very fast in this case. It is due to the solution being at temperatures where it’s not frozen, yet still cold enough to maintain it’s property.
- Place the solution back in a deep freezer.
- Wait for it to coagulate (“waxing”) again.
- Once it begins to clump together remove the solution from the freezer.
- Immediately begin the filtration process, we used the Hochstrom with a stage 2 (8 micron) chemical duty paper.
- Place back in the deep freezer & allow it to winterize overnight / 12 hours
See how the initial “rough cut” of the cloudy mass will flow faster due to different temperatures and separate passes.
Remove the solution from the deep freezer, if nothing clumps up & the solution is free of all coagulation you’re ready to move onto the next step. If you need to you can repeat the last stage of winterization as needed until you see results. Winterization is paramount to removal of unwanted compounds at different temperatures, allowing for much more efficiency in the overall refinement. The winterization is essential to do prior to this next step, or it won’t work.
Carbon Scrubbing & Polishing Extracts
Example: 1,000g Starting Material – 30% winterization loss = 700g Winterized Rate + 3.5-10% carbon based on the quality of the starting material.
Increase the temperature of the alcohol solution to 100-120f using the proper hardware & in a ventilated environment. Once the alcohol is at temperature add the carbon & seal it off. The Summit Research Carbon Powder A is extremely efficient in scrubbing unwanted & inactive compounds. Shake vigorously for 30 seconds up to 5 minutes.
Prepare a silicate bed & pour the solution over, this allows the Hochstrom loaded with stage 3 boro paper to flow freely when doing the scrub. This part of the process only requires a half vacuum for the Hochstrom filter.
Now you have a scrubbed solution.
- Roto evaporate out alcohol.
- When roto has clumpy extract with near zero alcohol introduce hexane or cyclohexane.
- Redissolve the solute into a new hex solution.
- Using a seperatory funnel, add the hex solution (scrubbed oleoresin) 1:4 hex. to the seperatory funnel.
- Take warm water and add salt. allow to cool but make sure its fully saturated.
- Wash hexane layer with salt water at room temperature. repeat this process untill salt water layer is clean.
Wait what just happened here?
In winterizing & carbon scrubbing you only remove oil soluble compounds in a solvent layer. The similar boiling points to curatives that come out during distillation are water soluble compounds – what are these? These attribute to the color : yellow, orange, reds, etc. When washing with salt water you get a lot of stuff that water attracts while the oil stays in the hex layer. This will refine a clear distillate upwards to the first pass & beyond. More steps are to be taken if you want to show off colors.
- remove hexane in roto.
- add some alcohol for transfer sake.
- remove all water, alcohol, terps, etc. so the solution is pure oleoreson that has been fully scrubbed and washed though-roughly.
- begin first pass at full temp, full efficiency, removal of entire body in shortest amount of time.
Collect this “first pass” distillate and now repeat a winterization process & another hexane, or pentane wash at this point. In the second treatment we find the most color reduction and compound purity results prior to the second distillation or beyond.
Now after the repeated winterization treatment of the processed oleoresin is complete, reload the machine & allow the spd series units to operate. In this short path distillation process you will now achieve deeper vacuum rates, higher rejection rates in the E-Vigoreux section & much higher purity results. This is done at a slower pace, allowing you to dial in how much rejection you want. The Summit Research unique process allows you to obtain high yields with just a single material treatment and a first pass. It’s where numerous distillation techniques come into play to produce guaranteed result. You’re guaranteed to add this tool to your bag of tricks.
This process allows the second, third, etc passes to be done at a faster pace, while the material dwels in lower temperature unaffected. High separation processes at higher initial first pass temps causes many more issues, thus resulting in the refined and precise protocol we have created to reduce any high temperature exposure times.