Are you seeing people trying to charge thousands of dollars to show you how to correctly perform pesticide removal?
Wow. Right. We have been selectively performing pesticide removal tasks that succeed, and pushing these processes free of charge for the public. In fact most of these writings are available in free patent articles. We have been preaching and selling these products for a long time – there is no need for some con man to tell you he has some patented method. Summit actually OWNS the patent for the high purity SOP (patent # US20170113160); this patent is used to clean up material, subsequently it does a fabulous job removing pesticides. So stop telling people somehow its a proprietary process. It is not, you most likely learned it from Elliot Kremerman. The patent literature beyond this relies on chromatography and separation techniques. Within this writing we will go over several processes to reduce pesticides and how effective they are considered.
General application components required:
Summit b+c carbon.
chromatography glass scale column. with back pressure.
solvents that do not mix with water i.e. hexane, pentane, dcm.
ultra low pressure nitrogen regulator.
digital automated flash separation(end of the line).
carbon long path drip filtration. CDF bed.
An example of using carbon in this method. Take a 3 or 4 inch spool approximately 12 inches long. Apply a very precise filter base setup with fine papers. A typical silica bed of even glass wool can be used as a preload. Different steps and measures are taken to prepare each one. None the less begin loading half way the larger carbon chunk at the bottom about half way up. Load remainder area with smaller chunks from half way up.
The next process requires a lot more attention to safety. It has been known to use different solvents in series. We do recommend just trying one. Hexane or pentane is used to strip the bed out from dust and dye into a discharge container. This can be safely disposed. you will now use ethyl alcohol and pour a hefty amount down the column until you feel previous solvent has been entirely flushed. Cap the column, but make sure it does not dry out; it is important to note that the carbon also should not be soaked, but plenty wet. This is your absorption buffer process. Without doing this to clean it out and pre-soak the carbon it becomes less effective.
You will now have a prepared column. Take a bucket or carbon with a siphon drip feed setup installed. Setup a drain below the column. At this process will eat up yields – it is advantageous to use this process with a 5000 gram drip load. not a 300 gram load. Begin dripping solution from top to bottom. Your goal is that NOT to perform this is a warm room – you do not want the alcohol to evaporate and take more yields. You want to ensure your drip begins at the top and takes 15 minutes to drip down. However many drips may seem like it constantly dripping, it can be hard to gauge this timing. Even a 10 minute travel path is suitable. But certainly not a 1 minute traveling pathway. These two carbons work in sequence and as it does rip out yields, it will rip out pesticides. Not as a final solution to a issue – but as a quick solution to bring extremely high numbers very low in relation to the results it provides.
It would still be wise to take this solution through silica bare, and then rotovap and re-distill. Considerable color increased occur when doing this process.
The next step is water washing. This can be done with virgin material that has been winterized, or this can be done with processed distillate. Distillate is much, much easier to work with. the example solution to be made up is:
1 liter distillate
1 liter hexane
2 liters of water
Either a water or a salt water mixture can be used. If your water already has a very high base content – adding salt might make it very hard and slightly caustic in reaction. It has been noted sometimes the pH would reside around 10, but the pH was changed so it would sit around 8-9. This allows the water to help release more compounds from the solution. using either a large reactor or a separatory funnel, load up the hexane solution first. If using hexane or pentane it would be wise to dip the temperature around 60c or lower to prevent the vessel to encouraging it to boil off vapor into your breathing space. always while doing this, you will have a cold trap hooked up to your separatory funnel – or your reactor, the reason being is while it is separating, it is also releasing vapors from the volatile solvents. The cold trap will prevent those vapors from coming out while it is sitting. repeat numerous water washes, once comfortable you can easily dilute the salt water back down, and repeat more washes. If you stop seeing crud in the water layer, it means it stopped taking said compound….and is now taking compounds you can’t see. This is why it is important to keep washing up to 5x past when you see the water stop taking things visually.
This step with water wash is very important as to complete the next step. It is considered a quick de-gumming process to prepare for chromatography.
Each step has certain things to offer, carbon has something to offer, and so does washing. This next step has a lot more to offer, but it is a high yield loss.
Prepare a column with half way full mag-sil, also known as florasil. Not all florasil works, there are certain materials and suppliers that actually do work better than others. Mag-sil is chemically a magnesium ion attached to amorphous silica. Again, the only type we have seen work out of the slew of suppliers is the genuine USA made stuff from the two pilot locations. They come with a specific sterility and ISO certificate from the manufacture. These are the only known ones we will suggest to us, a more passive version, that is faster, and little less accurate is sodi-sil, a sodium ion silicate. This will remove a lot more color, however little less pesticides because its a bit less accurate. So if your pesticide levels are high you can use mag-sil or if they are low try some sodi-sil at about 25% less cost. Creating the bed is tricky, typically you can compress it, or pour it in as a liquid and allow vacuum to compress it. Always add more solution to drain and avoid creating air bubbles. The point here it make a matrix of gel…like a combination of round legos that don’t want to interlock. The fluid flowing past these legos also has its own lego shape. The curatives generally will flow out while the small amount of pesticides attach to the florasil. See the trade name for florasil signifies a water based absorption for molecules and angstrom sized end chains in a microscopic level. When using a nonphobic solvent against it, the more phobic molecules will not drag past the material in a column where the solvent will take the oil based compounds, and leave a a lot more water soluble molecules behind. As we know harsh pesticides like Myclobutanil are water soluble. We have a high advantage as they tend to grab on and become left behind. As well as a reminder to flush the column it will pull everything out including pesticides, and this is why tossing the media is a common practice.
This practice can lose about 5-30%. The result with this process that summit created for the SOP on file with the USPTO for the schlussel key invention, was adapted for pesticide removal, and the target potency was 99+% d9 achievable with water clear results. With no d8 or further compound degradation pesticide removal was just a side note of the use. We initially used chromatography media in experiments and customer uses for clarification. It was then used with the key with incorporating water washes to fully ensure a effective and mechanical separation to be performed prior to re-distillation. The losses were not a worry as we were aiming for the highest grade distillate on the market with our SOP. The removal of colors, and pesticides was amazing, the cost to perform this step by hand is high, with huge losses encountered. Some material was less lossy than others and compounds left behind by this flash separation process cannot be removed with a single solvent pull. It is required to use multiple solvents.
This next step requires the use of a computer driven chromatography setup, also with water wash pre-processing.
…..not finished article. will return JBV