forms of pesticide removal

Are you seeing people try and charge thousands of dollars to show you how to remove pesticides?  Wow.  Right.  We have been selectively performing 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 – theres 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.  its 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.

sodium silicate.

magnesium silicate.

chromatography glass scale column. with back pressure.

solvents that do not mix with water i.e. hexane, pentane, dcm.

ultra low pressure nitrogen regulator.

filtration/vacuum bottle.

filtration silicate.

digital automated flash separation(end of the line).

 

carbon long path drip filtration. CDF bed.

a 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 alot 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 redistill. 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

::washed against::

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 cannot 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 alot 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 alot 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 dont want to interlock.  the fluid flowing past these legos also has its own lego shape.  the cannabanoids generally will flow out while the small amount of pesticides atach 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 alot more water soluable 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 degredation  pesticide removal was just a side note of the use.  we initialy 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

 

 

 

 

 

SPD-2 New Thermal & Packable Heads

New SPD-2 Thermal & Packable Head Technology

Here we have the new line up of SPD-2 Thermal+ standard & SPD-2 Thermal+ Packable. The concept is for the fastest packable head on the market with efficient increase in thermal properties. This head is designed for custom raschig rings we will provide with the head. The packing is lowered below the joint with enough plate indents to support it. Reason is dividing the packable section to the hottest portion while achieving a ceiling for vapor purification up top. This makes it extremely fast for a packable head and refuses to carry any of the unwanted distillate in the packed section. The kurzweg just got way better. Also SPD-1 & SPD-2 will remain as our legacy series in current production, don’t worry we won’t ditch our tried & true designs.

SPD-2 Thermal+
SPD-2 Thermal+ Packable Head

 

Short Path Distillation Procedure

Short path distillation protocol for operating the genuine spd systems for fractional distillation.  We have been consulting on this technique for several years. There is a lot of misinformation floating around on general extraction techniques & several others that will charge you for information that can be found here at Summit Research free of charge.

Step-by-step on how to operate the fractional distillation hardware properly

initial steps required for prep.

  1. winterization.
  2. scrubbing and polishing.
  3. removal of all solvent in evaporator.
  4. high temperature(140c) “punch” through all layers removing all water, alcohol, solvents, terpenes, etc..
  5. pour into load flask.

It’s important to understand why we do not use a transfer fluid like alcohol anymore, this will create a very violent and unstable foaming and bubbling in the short path apparatus.  To do this we typically place a large flask with 1.4 or less filled on a hot plate around 180-200c, this will heat up the large beaker.  allow stirring to be slow, and sometimes you need to apply hot air at top of beaker rim to facilitate the removal of solvents that would otherwise cool rapidly, re-condense and drop back into solution.  this process leaves the solution very foamy, this is why we blow hot air on the beaker rim to rip out vapor via thermal CFM push with a spark proof heat source.  do not allow surface temperature to exceed 125-140c.  we typically pull the beaker at right around 130c. As these temps to begin decarboxylation they are in no way whatsoever it is actually decarbing past around 1-3%, this process doesn’t take much time at all.  If you load too much fluid in beaker this will rapidly foam and possibly run over the top of the rim.  once you have removed all the volatiles, now you should have a properly loaded up flask to begin the process.

the next steps are incredibly important to follow.

  1. make sure pump has been ran, oil has been changed and depth is verifiable with a meter or sorts.  this is a opportunity to do a service. if issues arise run pump under vac for about 1 hour to allow to heat up.  replace oil, then run again for 30 min.  replace oil again.  this double flush process should refresh your vacuum pump.  if this is not the case and your pump is having issues please get a new one and overhaul your current pump.
  2. clean all glass joints as if you were to perform surgery.  everything from colt trap, to spd, even clean your lines if need be; replace lines if need be.  also make sure controller is clean and free from components lining inside.
  3. be careful not to use any hose laden with solvents or distillate as this will affect vacuum quality and performance.
  4. start assembling the glassware.
    a. apply a thing film of high temperature ptfe vacuum grease. this rating must be beyond 4-6 scale at 280-300c minimum for distillation protocols to be followed.  the result in ignoring this will be chasing ghost leaks all over your machine and affecting your process.
    b. the centered port on the Summit Research Triple offset flask is the thermo port.
    c. the offset port on the Summit Research Triple offset flask is the SPD head location port.
    d. apply grease on thermometer oring. tighten down, do not go over tight and ruin the material memory(under heat it will warm and smash on itself if you over tighten this part)
    e. insert the 14/20 head plug at top of spd head.
    f. position head so base of head is 100% even and upright.
    g. connect the monocow with a initial flask(250ml) for initial head fractions. at this time you should have another flask (500ml) attached to the second cow you were supplied in the set.  this second cow is the one that is spotless, and clean, readily assembled for the rapid swap that you will do.
    h. connect monocow gl14 port to lower port of cold trap.
    i. now connect cold trap to dv-1 throttling valve.
    j. lower section of dv-1 absent of valves goes to the vacuum pump.
  5. at this time you should begin to apply di/iso to to he ct-1 cold trap. below the trap in a dish as well.

You are now assembled and setup to begin the process of distilling cannabinoids!

 

Turn on condenser heater/chiller and set to 40-65c, we like 40c on first pass.

start up your vacuum system. allow a small leak to enter system preventing any initial boil over.  allow pump to pump but do not hit full vacuum yet.  begin adjusting all joints.  take note to the physical attribute of how the grease creates a film between the joints and ensure during this process the film becomes even while turning the joints to establish a full bite. now turn heat and string on.  begin stirring action around 200rpm.  start heat at room temperature, and start bumping up between 10-20 degrees C at a time.  it is note worthy that the slower you raise temps here the more stable the mantle will be.  during room temp all the way up to 140c this is the time this will be the hardest rate of temperature increase.  if you ramp too fast the mantle will not see the differential, and it will over energize the bowl.  this may over shoot in temperature and should be avoided at all costs.  stability in mantles increases the more you use them and the fuzzy logic pid  will gather data on heat and thermo probe information to calculate the accuracy and stability.  the more you over shoot, the more the pid will learn this, and continue to do this.  the less you over shoot, and the more stability you create from your process the more the mantle will learn this and continue to function on point.

As you are increasing temperature your leak will slowly be locked off.  The observation of this process is merely the result of action if the flask.  the more action and popping you get the more of a leak you need.  approx. between 80-120c you will see the flask contents reside as a flat liquid surface; at this point you can easily lock off the leak and begin direct vacuum control.

during this time you will notice if material is prepared correctly, you should see little to no fractions until 180-200c or past that.  don’t worry you don’t have a leak happening.  this determination of lack of reactions all depends on your skill level in preparing fluids to avoid all other boiling points that are unwanted, and the removal of inactive compounds within your solution.

even if you see some compounds popping in the vigoreux section, its not a issue.  these are all unwanted components. this next step is optional.  there are a few ways to perform this, we will start with the most basic way.   you will observe your cold trap, once all dripping stops you have gone beyond the volatile stages.  this means the trap is nearly unneeded in the process.  we see a typical removal of the trap around 180-200c.  this process is as follows :

  1. allow process to continue. when you notice a switch is required then perform these steps.
    a. turn off heat.
    b. turn off spinner.
    c. allow pump to run under vac for a minute or so(this will remove residual thermal energy from the mass)
    d. kill the pump, and begin bleeding atmosphere/nitrogen to break vacuum depth with the dv-1 valve setup.
    e. immediately remove upper port from ct-1 cold trap and now screw it directly on the cow.(this whole process takes about 4 seconds or so)
  2. now that you have performed this swap, you turn vacuum on first, and slowly dial out of atmosphere with the dv-1 valve setup
  3. dial in vacuum first, get to as deep as possible first while locked off, you may actually need to throttle the dv-1 valve setup.
  4. now begin the stirring action.
  5. turn heat back on.  notice, you should see temperatures ON POINT, or slightly below the set point.  during the time heat is removed, the vacuum applied creates a cooling effect on the mass.  if you took too much time to do this swap you have effectively allowed the thermal mass of the bowl to over energize(increase heat) the load flask.  if this occurs turn heat off and just allow vacuum to run.  if you are about 10c over for example running vacuum will take about 2-5 minutes to decrease 10c.  if you went over 10c, kick yourself in the face, you probably messed up bad and took too long to do the cold trap bypass.

i feel its important to add here.  don’t just do this process.  setup your machine with water.  turn it on to a low temperature, use a diaphragm pump for this.  and practice the monocow swap, or even the trap bypass.  just practice doing it all day.  pump on, heat on, stir on, and reverse, and repeat.  do this over and over until your swaps are GENUINELY short and efficient.  have a friend stand next to you for help.  if you are taking minutes to do something that takes seconds you are going to have a bad time.  practice makes perfect.

now that your cold trap is bypassed, you are at direct connection for the process. the only option here is to replace the cold trap with a NEW CLEAN trap with the LOCK OFF CAP, this will allow you to use a clean trap that has no fluids or sources for micro boiling effect that occurs under high vacuum and depletes the vacuum quality affecting evaporation in load flask.

now that you are at temp and vacuum begin to increase temperatures until you see your main cannabinoid body start to evaporate and saturate the head. we would suggest to allow full saturation to the top of the head to occur at this stage, the efficiency of this reaction in the e-vigoreux engineered pathway will allow all the clean compounds to flush out the pathway where the stinky and disgusting terpschwitz odors are laden.  you should see a sequenced WAVE like effect at the top of the condenser entry point.  this will fluctuate in effect but you’ll see the hot distillate flush out the entire pathway, sometimes spitting chunks of nasty terpschwitz compounds out into the first cow/flask.

now you will repeat the swap process, only this time you will swap out the good clean rebuilt flask/mono cow assembly. start simply by…

  1. turn heat and stir off.
  2. allow vacuum to dissipate energy in evaporation(subsided reaction)
  3. break vac, replace mono swap cow assembly.
  4. turn on vacuum, re initiate reaction in neck.
  5. dial in vig section as desired for purpose of distillation result(slow or fast).
  6. begin string, this will create more violent reaction, use throttling valve to dial it in.
  7. turn heat back on, if you are gathering a healthy fraction and set temp is higher than current temp, reduce set temp to right above 1c from current temp.
  8. begin collecting the main body and regulate machine with temperature and vacuum pressures as need be.  increase temps only slightly to garner different vapor pressures to evaporate your main body.  this is a very variable set points.  it changes with a lot of material.

you are now collecting your first pass main body.the rpm from starting at 200, can be increased as the mass of fluids decrease.  more fluid requires less rpm, as fluid(distillation occurs and output discharge equals less load rate) becomes lower the rpm can increase.  we have seen users go anywhere from 400-1800 rpm, however we like to see it around 400-900 typically.

imagine the main body from start to finish(no vapor pressure), now imagine there will be a 2/3 marker for the tails switch.

what this means, is you will be collecting the main body, fast or slow, however approx. 2/3 to 3/4 of the way in, you will see a obvious color change.  this means you past your hearts section and dove right into tails.  this is where odors and switching is difficult to control, you should have done the last switch PRIOR to seeing this color.  you will have the tails resemble a darker scorched honey like consistency, this will literally coat the glassware inside.  normal clear is more volatile and purer, it will strip the glass itself leaving a pristine no tint visual observation on the glass.  when the tails come you will visually see a tinted effect.  we always switch about 3 or 4 minutes prior to seeing this.  a explanation of what is happening here is the main body may be at 90-96% distillation output potency from the spd systems.  when this body comes it will itself be degrading in potency rapidly.  when you see it it may be 88%, and within 2 minutes its spitting 40-60% potency rates.  this is why your hearts is to be collected to retain the high potency rating. the tails to be collected later for reprocessing with other tails.

how is this done?  same way….kill heat, kill stir, kill vac, break vac…NOW ONLY SWAP THE BALL, leave existing mono cow attached.  now re initiate your process and begin collecting tails.   you can immediately crank temps up now and push out remainder of the product.  there is no need to go slow slow for this process.  this is just to gather remainder for future polishing and processing.

 

Rotary Evaporator Instructions

Summit Research Rotary Evaporator Instructions

please see diagram as this will show you basic link up procedures.

We have been educating & training our customers for years on how to properly integrate rotovaps with the process. We do not focus on low power packages that offer little to no recovery speeds. We’ve pioneered a rotary evaporator operating process that has made made progressive waves within the industry. What was once a long & arduous process of filling the flask & falsely spread information is now publicly corrected, here at Summit Research.

Setup steps:

  1. put rotovap together, remove all packing around coils with solvents, clean and make unit near sterile.
  2. connect cold output line from chiller to top of condenser coil body.
  3. connect output of condenser coil to the chiller return port.
  4. connect vacuum port from condenser to another trap(recommended to protect controller).
  5. connect trap to controller input.
  6. connect controller output to pump inlet.

operating steps:

  1. turn on rotovap, set bath temperature from 35-45c.
  2. turn on chiller and set temperature to 0-5c
  3. turn on vacuum pump and set your controller to right above the cusp of the evaporation rate(generally 100mbar).
  4. allow both coil and bath to reach temperature while vacuum is set and equalized in system to set point.
  5. now set vacuum approximately 15-20% lower after everything has reached temperature.
  6. now feed in small amount of fluid
    a. 5 liter roto 100-200ml
    b. 10 liter roto 100-200ml
    c. 20 liter roto 200-500ml
  7. now allow the beginning of the evaporation process to occur.
  8. watch the discharge side, during this time you will se a rate of liquid recovery.
  9. start feeding liquid into rotovap slowly, match the inlet speed to the discharge side of the rotovap.  what is coming off the condenser, should be 1-3% more than what you are feeding to rotovap.
  10. very important here – Dip the vacuum down as low as you can go, while watching both the condenser and the trap. Manage vapors to remain in the rotovap and not bypass the upper vacuum port.  Ramping down vacuum should be done only after the initial dial-in is achieved as this will increase heat loads exponentially to the chilling system if not done correctly.
  11. allow the feed line to continually pull from a storage bottle of sorts. replace bottle as needed.
  12. this process can be ran nonstop until desired amount of goop is in the evaporation ball and the efficiency of evaporation is decreased.
  13. empty the solvent discharge ball at the bottom of condenser as needed through process. only empty evaporation flask when as needed.

This is called batch feeding the rotovap, you will be able to achieve the fastest times possible with this process.  Note that any weak or inefficient hardware will either over heat, or stop working properly if you choose to go down the route of using the wrong / mismatched gear.  this process requires a inept understanding of how to operate nonstop and being able to match up the components.  Summit Research has done a terrific job at pioneering this process and matching correct components up.  if you require even faster speeds – please contact us for custom solutions we offer to large scale labs.  questions on more advanced processes? Contact us or visit our showroom in Scotts Valley CA. to view the latest & most efficient innovations & exclusive equipment offers.

 

 

Advanced Short Path Distillation Techniques

Short path distillation techniques have advanced tremendously for the cannabis industry. It’s important to have a basic understanding of the process 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 seperate 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 cannabis 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 gaurunteed result. You’re gaurunteed 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 seperation 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.

enjoy!

-jbv

Fractional distillation protocol for first pass main body collection.

In this section we will focus on something not so common. First body removal. The actual boiling points used in isolating specific distillation output can be very tricky at first. And sometimes nearly impossible to gather through a short path head without massive trails on contamination. Hence the difficulty of distilling cannabis through a thin film requiring numerous passes. This can be simplified with a mantle and the process can be dialed very well. As a mantles create vapor pressure from operation and other distillation hardware does it. It funnels vapor molecules through a complex and contaminated path(if not rigorously cleaned between flushes) when using wiped film and thus the requires passes and numerous processes are needed during isolation between the different boiling points. To be clear we may see a average 220c temperature calculation of the true boiling point of cannabis as noted in the 1960s patent filed by two Israeli fellas. These were noted and explained in detail that the boiling point reached each time the components were fractioned out and tested was lowered and inherently higher during the initial pass. Do not take temperatures to heart on the head or anywhere other than the load flask. We have seen anywhere from 230-260+ required to make the initial pop. Here we will go over basic processing steps to get the cannabis distillate out. When reading your distillate you can create a ultra clear extract and manipulate the bp on the second pass because the molecular density holding everything together has been lightened up dramatically. The initial fluids will hold alot of the components you are removing with a tension that reflects the heads and distillation performance. Where the curve is seriously altered after the initial body has been removed you are now able to dial in less temperatures, up to 50c less, and use different types of pumps to create different effects and results.

Preparation for the first pass –

To begin we suggest using hardware to duplicate this process. Without using the exactly hardware your protocol processing steps will be all over the place. Replicating a using components designed for proper operation of these processes is very important. Using cheap chemglass, or lab boy glassware will always serve the user with issues. Short paths, crappy glass, leaky glass, etc and so forth. In our testing we have achieved the PERFECT and absolutely precise design of where the molecular distillation of cannabis is to reside. In the spd-1 e-vigoreux head. The first and only cannabis head to ever be released, specifically tuned for our environment when distilling.

It is very important to notice the distances, and the shape changes. As there were mathematically calculated to reflect the “earth based distillation”, the the volatile compounds distilled in short path heads. There ARE NO stock heads on the market made to operate in the way this distillation is designed to work. That is why we stand behind this head and guarantee repeatable results with higher purity, and greater efficiency in operation.

The protocol for the first pass of fractional distillation –

The second most important items on this list is the correct mating of hardware. We use a digital mantle and offset flask to guide the vapor in the right way, and also keep your thermometer correctly positioned until the load flask empties. The same goes for out mono swap dc-3 cows which eliminate all contamination between fraction switching. We will talk about how and when to use a cold trap for this process, as well as how to work the vacuum. Do not kid yourself. If you have not done this before – and want to enter on a budget, you will be shocked at how difficult it is to operate the setup in a efficient manner and get repeatable results without the correct hardware.

Cannabis distillation, efficiency rates based on engineered specifications for production/purity shelf operation.

SPD-1 technical op-sepc.

  • Output: 430 grams in 30 minutes.
  • Range output based on mg content: 300-450 grams in 30 minutes.
  • Initial tail removal and temperature sequencing with vacuum: 30 minutes max.
  • Conversion and efficiency rate: 99%.
  • Total elapsed time from start to finish: 1 hour maximum.

Variable experienced time due to inaccurate temp and vacuum sequencing: 1.5 hours maximum(should always be avoided and practiced sooner)

one thing to remember is that THC will degrade, the temperature wont be a enemy as the time dwelling at that temperature is the enemy. 240C for 2 hours is the same relative degrading rate as 260c for one hour. This is a example per volume load. This is not to be quoted. It is to explain the difference and those times of degraded rates of the components we want to remove are actually highly variable.

This information is a guide to prevent you from dwelling your extract too long. The concept of cannabis distillations to retain yields and quality and high potency numbers is solely based on how fast the thc main body can be removed once the main body pops. And long term dwelling or temperatures that sit too long between fraction separations tend to cause contamination.

Now we begin the process of sequencing the vacuum and temperature to ensure we push out any contamination and unwanted odors or components from the load before collecting the main body. This process smells like Auschwitz. Myself as a individual who was learning, the fist two times were so bad I vomited and almost gave up. Within the tenth time i was so good at isolating this odor and removing it, my students were shocked to barely smell it. We had to show them the flask itself to learn what that smell was or else they would not be able to identify it – and prevent it. But i will never comment on anyone inability to do so as it is very tricky and requires a fine method of operation where no mistakes are made during the sequence.

The initial sequence is followed in a “two steps forward, one step back” tech. Note with temps and during main body tuning this is the rule of thumb. For the temperature we will set it to a desired number and far before that number is reached we will increase the temp. Do not ever set your mantle to say 240c and walk away. The digital systems now a days may keep temp, but do not sequence it. This sequence is based on a 600-800 watt mantle for 2l, and will suffice for a 5l with a “double rate” by volume increase in wattage. Example, a 1000watt 2l litter mantle needs a further rated sequence with a enlarged bandwidth increased before vacuum can follow along with temperatures. Int his case we are talking about a standard medium wattage high temp board pid control. Our 2l and 5l mantles all follow the doubling rule when we have them made to spec. This also matters how accurate and responsible your thermoprobe is. For sake of education and operational guidance this is revolving around our style of mantles. We have yet to find a affordable version by any other company that has the correct ramp speeds added, and thus not allowing a digital unit the ability to screw up the process of sequencing the temperatures and vacuum depth so this is to be done by hand, an the results speak for themselves.

MANTLE                 TRAP                  HEAD CONDENSER

60c                            ***                                0c

100c                          ***                                 –

140c                          ***                                 –

180c                          **                                   –

220c                          *                                    –

230c                                                             40c

240c                                                             40c

250/260c                                                      40c – (up to 50c avoid if can)

this process should be observed that when we set it to 60c, and the temp is 10c away from 60 we set it to 100c. When the temp is 20c away from 100, we go to 140c, and we follow that 20c chase rule until we hit 220c, and step 10c one after the other within 1-2c away from orig target temperature. 250/260c is relative becasue depending on the molecular density, and the load flask ability to release desired boiling points this can vary. We have seen more efficient reactions with 250 with some material, vs 260c as a common go to temp for nearly all the material we have handled.

***

**

*

this is the sequence of use with a cold trap. The actual numbers and temps here vary considerably. Cold trap is to be used during the initial solvent removal stage and along with any other volatile compounds that are being removed. However when the vacuum in the load flask is depleted becasue the cold trap is slowly releasing atmosphere internally from boil off it is wise to disconnect the cold trap. Slowly dump the vacuum in the system and quickly swap the threaded ends from the top of the trap to the cow and restart the process.

This is a guide and not a exactly sequence as the sequence itself changes with every material you run slightly.

The vacuum sequence will be as follows:

MANTLE                  VACUUM % RPM

60c                               30%

100c                             30%

140c                             50-75%

180c                             50-75%

220c                             75-100%

230c                             100%

240c                             100%

250/260c                      100%

this is very tricky, and normally only be done with a vacuum control valve and a aux valve used to pin down ultimate cfm on vac. Not ultimate vac. The easiest but hardest way to acquire this process is getting a variable frequency controller. Without on you may need to use a series of needle valves and atmosphere bleeding valves. Note all series valve hosing to be used on a displaced manifold, so if needed the link can be entirely removed from the hosing circuit and adapted to direct vacuum control with one regulator(if needed).

The process is as follows for entire fractional distillation of the main body, however note that base on vacuum performance, and user experience these numbers can be altered. This is a basis to teach you how to do this. This is basis to learn and it should be followed precisely and thus can be altered after the entire grasp and ability to control each factor has been mastered. Once you move outside of this process with hardware variances the entire process will vary dramatically but the over all operation and mechanical performance itself will be near identical. Just the process protocol itself will shift from either direction on a sliding scale.

First make sure all glassware joints are cleaned to sterile quality before assembly. Possible use of grease is needed for new users. Do not ever attempt to switch the cow or turn any glass while at vacuum. If you have a issue shut it down, and kill the heat. Yes the alcohol will continue to boil off and most likely degrade the clean joints and load them up with earl and all kinds of nasty stuff. Disassemble the unit and let cool back to room temp, both glassware and mantle itself or else it will force this vapor up and contaminate and ruin the clean joints you have. Bad joint health will lead to failure and or depletion of vacuum or even welded joints and broken glass.

Now while you initial temps are rising you will set 200rpm, and this should be enough all the way to 2/3-3/4 of the main fraction body you are removing. Then you may raise the rpm to 400, and then to the end 600. this is only needed to basically splash and move the fluid up on the glass to get a more efficient boil off when the load flask is low and the vapor pressure provided is not entirely powerful enough to generate a reaction. Over head stir or wipes are relatively useless when it comes to cannabis distillation as the performance curve is established with the ability to generate vapor pressure under vacuum. Treat the pill, a small pill is all is needed to create the proper spin. Do not get a crazy sized pill as it is not needed and can diss-balance and throw itself around causing the glass to break. You are better off using smaller stir bars to not dislodge or damage your thermometer probe. This is why our setups come with stainless probes to prevent glass probes from shattering as well.

Beginning the process of distillation will start with removal of solvents. The cold trap will be spitting solvent at this point, do not attempt to control the condensing rate in the head itself. Allow the 0c set temperature to actually do what it can, condense some alcohol and the rest is vapor to allow the col trap to condense the rest. If you use a variable freq controller start off at 30% and with the regulator basically breathing, by watching the fog in the cold trap you will be able to control how much of the regulator is dialed in. Too much fog coming up to the vac port – open regulator, too little happening in the cold trap – close regulator. This needs to be accomplished while also tending to the load flask reactions. It can sometimes be violent. But you do not want it to look like still fluid. You want to see it bubble and bounce a little. This means you are entering each reactory phase. If it is still and vacuum is deep, it is a indicator of a leak or a more serious issue. However do not let the reaction bump past the neck. If it does whatever went past that neck is basically garbage – you are welcome to disassemble the unit and reload it back in if you screw this up. But that takes time. And it is easier to abandon that little 50ml of fluid so to speak.

During the time it takes for all the alcohol to evaporate your vacuum levels will need to go deeper. Around the time where the alcohol looks like its gone you will not only increase the depth of vacuum but now start ramping the variable control on the vacuum pump up.

During the initial distillation of more volatile compounds you will notice that the reactionary effect depletes itself and now stuff will be boiling out of the cold trap. This is a indicator to shut down the system and switch the vacuum line from the cold trap directly to the cow. As well during this point you’ll increase the vacuum control to 100% rpm while still re-engaging the vacuum depth as needed to begin fractioning out the initial non volatile compounds.

We suggest around the time you are doing he bypass from the cold trap you will already have timed out the system to apply 20c temps on the condenser. This timing is crucial or else you will simply cause a blockage. Vacuum will die and maybe even pop the head off the load flask if pressure persists. From the moment the solvent is distilled along with volatile compounds to beyond the moment you do the cold trap bypass you are already preparing the chiller to rise to 40c. From this point on your temperature will eventually match up to 40c on the condenser and level out there by the time you hit 220-240c. This is crucial as you are not only sequencing everything in vacuum stages but temperatures and without aligning this process correctly you will immediately run into issues.

In turn, BEFORE the thc main body hits – you will be at 40c approx half way through the initial tails where all the nasties come out. Those smelly components are everything from terpenes, to chlorophyll, plant dyes/pigmentation, waxes, fats, lipids etc… you must already be at temp at the neck condenser before, or else these thicker/harder components will load up and clog the neck.

The amount of tails is very dependent to the product you are removing. We have counted anywhere from 15-40 fractions on average will boil off far BEFORE the thc main body starts to boil off. A indicator of this presence being the garage is that the reaction is the neck will increase, and decreases or even cease to exist. This is the boiling point that ends. When thc or main body hits it should be the highest % of boiling compounds present. Meaning IT WILL NOT STOP until the reaction is entirely over and you have depleted the vapor pressure avail to create this process and sustain it. If you think you are at the thc. You probably arent. The initial components once close to thc look very similar. But are very NOT similar. Wait. Be patient, if you are on the main body allow it to run for a several seconds to clear the pathway and allow it to self clean. When you switch the glassware out this will prevent cross contamination and odor issues. If you think you are on the main body, and you do the switch. Then re engage the process and then the fraction dies on its own 2 minutes later. You were not on the main body. Again – the main body once it pops will not stop reacting at all until it depletes the compounds that are available for the reaction itself. This can be tricky and you have no contaminated your batch. This is why being patient matters or expect to buy lots of extra glassware to accommodate for these mistakes as cleaning and maintaining the glassware IS NOT A OPTION HERE. You will over extend the dwell times and ruin your output product. These switches must be done very very fast or else your mantle or any heating system on any distillation apparatus will over shoot temps as the evaporation creates a thermal condensing effect and self cools the hardware.

Now comes the very very tricky part. Using a series of cows, or even a tree port cow you will have to accomplish a switch. Even if it means taking off the cow and capping off the other two sides and moving it to the opposing side to isolate contamination or using our mono-cows for rapid switches and completely isolating any contamination that may persist through a system. The notion of turning your cow is a myth, dangerous practice and should never be down under vacuum or operational load. This glassware, and the necks get very very hot and even if it did not break – and the load flask broke under vacuum it will throw 450f fluid all over the place. This is not fun. Remember there is only one correct way to do these series of steps. We feel like going outside of this, not only is bad, but not worth the time to have a issue and then have to relearn it again. Once the thc main body hit you will allow the path to clear itself. At this point break vacuum and allow to disengage the seal on the cow. Remove the cow and either replace it with a clean set of glassware, or remove it, and cap off the other two sides and move to the opposing end and reinstall it.

At not point in time should you ever be collecting the main body thc while allowing other receiving flasks on the cow to hold the tails. This will continually contaminate the surface of the clear. As these tails do boil off as well depleting vacuum performance and they are present. As a example if u think u can smell it in the flask – it must be removed. No questions asked.

The practice of not removing these spent flasks is astounding and we see people doing it all the time on facebook and instagram and we cringe.

The whole concept here is to isolate, keep clean, and make sure you stride for the best process protol you can get. Each run yields thousands of dollars at times. A excuse that a lab cant afford a few hundred dollars in spare glass is ridiculous. Ludicrous!

This is a very difficult part to do here. After switching the glassware. Your vac will be direct by now, long by now….and the system will be void of all contaminated glassware/surface area and replaced clean. Vacuum will be turned on while the regulator is breathing. And the process will begin to restart. This section is to explain how to control and restart the reaction. With the slightest turn bring your load flask to a slight pop/boil, nothing dramatic. This will be spinning at 200rpm and it will seem sort of poppy. Slowly begin raising the vacuum depth. You will begin to see a “over reaction” in the boiling flask with a high boil. Avoid pulling through neck. The trick to this is two steps forward, one step back. You will continue to drive the reaction forward, and every time u move a hair forward on the regulator – you are to move half a hair backwards. This will create the alleviation rate response. There is a threshold where everything looks like it will explode. But not really. We want to go beyond that. How you say? Wont my nix just get sucked up? Yes and no. The reason behind that loaded question is, if you can pull a higher vacuum than what can boil off in a reactionary state; to resulting reaction thereupon is the loss of the “overboil reaction”. The actual process of alleviating pressure further than it can be provided will entirely “overboil-react-drop” this will pull the reaction beyond its ability to boil and the fluid will entirely drop. Think of it like warm purge muffin tech. Where the muffin rises and drops instantly after and just turns to a slab. In the same instance you will find the vacuum pressure seems bad and powerful. If you keep going it will nearly immediately look like its going up, then down, and then back off and level out. The fluid itself will flatten and just look like the spin bar is moving with small bubbles. This is the decarb effect and its loosing the C-OO, or co2 portion of the molecule. Right now the vacuum pressure and alleviation rate is so high that the gap between the head and fluid of the load flask is PURE hot boiling vapor. The reaction will now become more violent and powerful in the head. Gathering in the head and creating the distillate flow. Without crossing the threshold you will immediately lose efficiency until that point. This is the point where efficiency is created in the reaction. The only issue is, with a chemglass or short stock heads the space and gap is so small that the rejection rate is not accomplished.

Here we talk about identifying features and results of operation of mantles. The distance between the load flask and vig is the gap of vapor where pressure is derived. The vig section is designed to create a heavier condensate reaction, and as the molecules are hot and separate, but react they will reject and send back the heavier even higher boiling point compounds while the lighter ones come through and pass through the vig reaction area. There is then the effect of gravity that is void from most other systems. Also consider the purity shelf in our heads both brightens colors and increases potency and efficiency – something no other heads do. We like to think the perfect math can be done to achieve a basic reaction and result. This is backed with side by side testing of different sized heads that all operate in a non efficient manner. This is why we are adamant about making gear designed specifically for performance.

These topics we threw in here is to show you what we as lab workers look for. Without understanding those concepts it can be difficult to run a short path. There is no such thing as set it and go. You really do need to watch and understand what is happening. Understanding what is happening and how to control it will fine tune your skills exceptionally.

During the collection of the main body at the first pass you will enter a moment where the reaction is occurring, and the condensate is dripping all clear. Base your reaction on either 1/4-2/3 reactory effect in the neck. Beyond this is okay, but it is considered high production output style, with less separation power but extremely high output ability. In many cases you can tune and run a spd-1 with that high output processing capacity with outstanding colors and still be void of flavor and odors.

While you tune and get the reaction to sustain itself during this time, and only this time you will reach a “hands free point” and nothing should be touched or altered. Like we said earlier – once the main body hits, the pressure from vapor boiling off will be so high and intense that you wont be touching anything and it will just pour out. That is how you know what fraction you are onto of. If it dies, then you have 1% of the body in those crap distillations, if it sustains then you have 99+% of the body during the distillation. Again you can tell with how violent and fast the reaction occurs. This is the main portion you are removing.

In the near minutes after the reaction subsides you can crank up the pill to 600rpm and splash some more fluids on the glass sides. But the reaction will eventually die. This is the indicator your main body is complete and you need to shut the system down and disregard the rest. The defining point is when the bright clear reaction in the neck turns darker orange. This is the last of the cbd, cbg, cbn etc components. It will also coat a orange tint to all of the glass. This is the indicator you can switch it out sooner and collect this darker stuff in another flask. Or you can continue until the reaction dies. We prefer to take it till the reaction dies. This way we get a fully activated and wide profile distillate that is nearly 100% bio available.

We will return with more information shortly, we are working in office, brew on this we will complete the process….jbv

7/6/2016 we will be adding a new update to distillation processes, very shortly however we are busy writing up proper updated filtration and distillation procedures as we are releasing products faster than users can respond.  thanks and look forward to the new shit you will be seeing!

7/11/2016 updates hardware package for success. Updated procedures.

First off we love to say in the past times we thought we had it down. Nah. Now we have shit way down. The goal was to use the kown techniques, and processes to gather a control. And learn how to expand. We can outfit labs now and produce 40lbs of clear in a day in no sweat. So lets get you on the path to sucess. This is the list of the most comon selling package and what it entails. Then we will get into what we have been doing different for the istillations. And how we are controlling it.

  • 10l across international roto
  • Polyscience chiller, either 45l-25 or 15-40 ad models. (we no longer sell other brands due to common issues we want to avoid with customer purchases :-))
  • 4 head diaphragm vacuum pump, with even a jkem control, vacuum control on a solenoid valve will work.
  • Summit exclusive vfd edwards 30.
  • 2l spd-1 e-vigoreux short path distil kit.
  • Summit swagelok distillation solution.
  • The original sondergut silikate pulver.
  • Summits carbon solution.

This is a kit to sucess for colors, and reduced fractions to obtain the best quality possible.

The 10l rotovap is the next step up from the basic 5l, and recovers twice as fat with proper controlls. Also the uber benefit is less time needed. U can use a larger chiller and RIP it through much faster than just 2x the speed. Its a durrable unit!

The polyscience chillers are made in usa and made to order unless you pickup from our store stock. We have had ZERO issues with these unlike most any tempermental chilles on the market. But hey, its not a sales pitch. We just dont want to see you again over a chiller in the future.

We NO LONGER endorese cole parmer vacuum regulators. They arent the best, but after over a year of being loayl we say as a entry method it works. As a solution for future it doesnt work

we now sell a three valve manifold wich allows nitrogen flow controll, distillation controll, and ultimate vacuum throddling. This si teh best valve setup weve seen to date. And our part number from swagelock mimics the package we provide in quality. These will come sealed and they will give u endless use without any rebuilding needed. However it can be rebuilt, washed, re assembled and you just need seals. So this new swagelok package is trully a step up in the game of distillation controll.

Heres the kicker. We get a exlsuive buildout and customization package for edwaards 30 pumps. This will really let you control the distillation parameters.

We take our rebuilt pumps and we scrap the motor since it will not suffice this kind of abuse. We then order a brand new USA multi freq motor and have the shlaf shaved down, shortened and notched to fit the coupler on the edwards 30 pump. This is not common and is 100% custom. We will include a TOP OF THE LINE SPARED NO COST vfd digital controller in the package. This is a no brainer. Get it, and enter the future of vacuum distillation controll.

So all in all we have a deailed list here, other than lab stands and hoses, plus some basic hardware you will be ready to dump out lbs upon lbs of clear in a day with a basic 2l setup.

so. what have we changed? Not much, we still run machines like champs but we ran into a few issues, so from here on out this is a basic informal bench of what we follow.

  • Winterize.
  • Repeat untill epic no coagulation.
  • Carbon scrubm – with matrix mixed.
  • Silicate srub the solution from remainder dusts and final polish.
  • Nothing, i repeat nothing gets touched without being fully dewaxed and scrubbed to the max.
  • Roto down.
  • Decarb rapid to 150c to degreen the intitial stage.
  • Put in load flask warm, not super hot.

Go for it.

We are releasing some more stuff here in the near future, please feel free to contact us on anything you need or if u want to see more info updates in this section.

-jbv

Proper Distillation Procedures and Cleaning of Hardware.

Ever wonder what happens when you get a rst back and see there is iso?  This is triggered by 4 different isomers at times.  But generally an alcohol one will be present if you use alcohol to clean your gear and do not allow it to evaporate. The use of alcohol, especially with cheap ethanols, is a mixture of denatured components.  We suggest you use 99.9% denatured clean-room alcohol.  It is denatured enough to be cheaper and not taxed but its nearly nothing.  We prefer Pharmoco-apper clean-room.  It is cheap, and is non-residual, so it leaves nothing behind.  We also suggest after each cleaning, when you clean the inside of the vessel, that you also use nitrogen last.  This will help dry everything out.  We suggest nitrogen because even after the end of the day you can flush your clean vessel with nitrogen, which is sent down the path to filter drier, pump, coil, and out the recovery hose.  Essentially, you can dry the whole path out as well.

The concept of distilling fuels is completely missed when people think the desiccant drier is there to do the work.  No it’s not.  It removes lose chains in the pathway of vapor, which captures molecules that are heavier and whole in the hydrocarbon passes.  Foreign solvent will get caught but not in a direct stream.  The drier will only capture the denser molecular solvents while the lighter ones pass.  So if you are distilling and the majority of the gas is butane or propane, then things such as terpenes, alcohols, esters, pentanes, etc will be caught while the majority of butane or propane passes.   When you are distilling down your system, there is a point where saturation of the foreign solvents is enough to excite them and carry over during distillation.  The solution is one of two things: cut distillation down above 0psi, carbon bed(disposable), or clay sponge powder.   In the simplest way possible, you don’t need anything but cutting recovery short of 0psi.  Normally, if you have a 10-12 inch bottom, you would want to leave about an 8 inch puddle minimal at the bottom.   You will see the butane or propane bubbling, we prefer larger puddles.  When the bubbling decreases and the liquid is thin it can be an identifier of foreign compound saturation limits.   Typically if you are running around 100-110deg f, you should see an 8 inch puddle around 5-8psi with a 70/30 blend.   Shut system off, lock off desiccant drier, and bleed pressure out of your vac port.  You may now open and clean out your system.  If you smell any unpleasant odors -that means you did the job right and left it behind.  If you recover too far down – and don’t smell much but just see mystery oil, well, you may have carried over your residual components found in foreign solvents.   Avoid using Power 5 or Power 7 or whatever-13x, nobody cares.  All of that is the same when it comes down to foreign solvents.  Even puretane canned butane has pentane in it.  The x rating can be relevant to the amount of mystery oil, but that doesn’t mean anything.   If you start with a 96% grade Power 5, even with a new desiccant, that should be discarded after first distillation. You’ll only get 1% max cleaner fuel each time and no matter the times you scrub it, the end result will always be the same.  However, when we talk about fuels similar to a Praxair 99.95%+ or Eco-green 99.97%+ source gas, a desiccant drier can easily take it to 99.99% in one pass.

 

if you think we need to add anything to this please let us know.  we want people to be doing these tasks correctly  summitindustrialsupply@gmail.com   -JBV

Basics to Fractional Distillation

First off, very first, we emphasize, ABSOLUTELY ALWAYS follow safety precautions. Do not try this unless you are an experienced extractor or if these technical skills presented below surpass your lack of knowledge. This is not to be taken lightly! Wrong moves make glassware implode at full vacuum within temperatures of roughly 500 degrees Fahrenheit. Knowledge is here. Experience will determine failure or success.

The hardware required to complete a proper clear extraction is very complex in addition.  Like a puzzle, if one piece is missing or poorly supplemented, the system will not generate proper operation.  We are not looking for a vacuum depth as much as we are looking for a reaction in the short path distillation head. So take into consideration that you don’t need a vacuum gauge.   The basics will also require a fine, relaxed emphasis on rotovap work.  Like a CLS – we’re recovering alcohol. We aren’t aiming to ruin or lose our alcohol.  We’re aiming to safely and properly use hardware dedicated for each use.  I will explain in depth what is the ABSOLUTE BEST SOLUTION for both quality and performance.  WE HAVE TESTED VARIOUS METHODS AND HARDWARE.  We know what will create a proper vig reaction.  And what is barely achieving, thus ruining the batch from improper timing and temperature variations, essentially scorching the end result.

When working with fine compounds using the hardware we supply for perfume manufactures, you must use vented hoods as excited solvent has vapors, which is carried over during extractions and with floral collections.  This solvent may still pass through in high volatile vapor  form.  The condenser and cold trap will capture say 99% of what can condense at those rates.  As such, vacuum operation will expel low amounts of flammable gas.  For example, look at how limonene is made.  Several solvent bases have vapors that are harmful.  When using the hardware at upper limit temperatures for lotions and bases you are boiling out solids, or what are solids in excited form. Then they condense past the purity point of the short path, and based on condenser control, you can separate discarded gases and collect desired condensate.  In the aspect of cannabis extraction, you must remember protocol to make one thing for lotions or perfumes or even food grade flavoring, it is not the same when obtaining a solid acetate.  Solid acetate is the process of boiling out a solid molecule until the boiling point is reached and a steady head pressure of vapor develops.  This whole concept relies on the heads ability to maintain that temperature and to “over condensate” the heavier compounds and reject them from the vapor path.  The upper most volatile vapor pressurizes is typically knows as a slag ceiling.

In the comparison between a typical head where the slag ceiling is present and the E-Vigoreux SPD-1 where there is no slag ceiling we can direct the path in the function we need.  At first your collection, based on control factors, may contain the high purity excited vapors that condensate and also collect some of the condensate that reacts in the vig.  This is fine.  On your first conversion, the molecular weight is so extremely volatile in either direction of vacuum pressure that you will only collect a profile subsequent from what can be loosened from the heavier molecular bonds present in the load flask.  If the compounds are poured into the load flask, the boiling point re-pop will be with finer control.  Meaning you can actually create separations where the BP will not “group react” with similar ones on the first conversion. Comparatively, the purity shelf is considerably higher on the SPD-1, which allows for greater initial control due to the re-engineered path initial suck up that has been prevented by 75% from what I have experienced (sometimes maybe even greater).  We can cross the bp vacuum pressure thresh hold faster and create a reaction that will cross the vacuum pressure median.  What this means is you need to create a slight over reaction, and continue this process until the vacuum pump catches up and crosses the threshold for the reaction.  The initial suck up effect must be achieved first, and the vacuum gradually is increased deeper and deeper and thus vig vapor condensate reaction and rejection occurs.  We can discuss what the reaction is and other principles at a later time.  This is to understand what hardware is needed to do this process.  Hence….if we can make this work every single time with no exceptions while others who start and do not have success, it must be attributed to cheap and slightly under powered hardware.  So thus, we say, get the best of the best.

  1. Huber unistat 360 chiller/heater.  Ethanol fluid
  2. 2000ml digital mantle with stir features. 5Liter probe, built in pid control for probe.  Do not buy separate control units.  You’ll thank us later!
  3. Rotovap with vacuum control and a dual diaphragm balloon vacuum pump.  We like the i100+v700 Buchi combo.  We hear a standard r100 Buchi will get the job done exceptionally. 20K rotos aren’t a need.  You need reliability and control.  Not ridiculous branding.  Your work will only be as good as your rotovap.  Keep that in mind.
  4. Cold trap.
  5. Short path head and round bottom flask with attachments.
  6. E2m30 or 2021 style vacuum pump.
  7. Cole Parmer thumb vacuum control.
  8. 90mm modular filtration apparatus.
  9. Glassware, beakers, filter flasks, separatory funnel, media bottles.
  10. 5u filter paper and glass wool for biological filtration.
  11. Numerous lab stands and lab elevators
  12. 100ft 1/4″ high duty low and high temp silicone hose clear.(this will let u identify issues carried over in vapor path) and use in everything from chilling to vacuum.  Fractional distillation ruins hoses and coats the inside with a deathly odorized product we just throw away.
  13. Digital head gun
  14. corning pc-620d thermoprobe kit heat plate. With spinning control.  Digital.
  15. PTFE stir bars and long stick PTFE retrievers.  Cleaning brushed for mantle flasks.
  16. 200 proof ethyl alcohol non denatured.  Lab grade HPLC cert.
  17. One flameless digital e-nail to keep you company while you are rotovaping.

this is just a introduction, if you think we left something out, and want anything added or talked about here please email summitindustrialsupply@gmail.com and well be happy to add relevant into.  -JBV

Fractional distillation of cannabis – basics series 1 of 4

Introduction to the beginning basics of cannabis distillation, including terpenes, thc, cbd, and all related components. this is a intro, how things work and basic knowledge needed to understand the process from 0-99% minus small details – which we will include in questions answered and update video for more depth. This is part of a four video series to bring people up to speed with the best processes available.