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Tek THC Distillation

EugeneOregon

New Member
Here is the purification method used on the extract prior to molecular distillation. It uses a combination of first dewaxing through a short column of aluminum oxide while disolved in alcohol which removes waxes completely then codistillation of most of the alpha pinene away using water and simple distillation. Following that the extract is recovered in hexane and water removed by employing a seperatory funnel. Then chromatography is employed to obtain a high purity fraction ready for molecular distillation. Each step refines the extract further and when used in concert together can yield nearly pure delta 9 thc.
 

herbivore21

Well-Known Member
Welcome @EugeneOregon! Very interesting videos and thank you for such a bumper first few posts! :biggrin: I hope that we will see more from you!

One thing that I want to point out for other readers (@EugeneOregon is likely to be aware of this already) is that vacuum distillation is not for the uninitiated. Those who are watching should not try this at home/anywhere, unless they have the requisite organic/analytical chemistry lab training and knowledge. Missteps during distillation under vacuum entail risks of glass implosion, hot fluid injuries etc.

A few points of discussion I'd love to chat about with @EugeneOregon:

Edit: Never mind the original first point, it seems from watching your video with the chromatography that you have a pump with PTFE internals which likely renders what I first said moot. lol

2. Also have you considered the ready made claisen adapters which in some cases come with a thermometer, and in any case provide for you to use a thermometer inside the sealed vacuum environment, measuring the temp from inside the distillation path, rather than around the outside of the glass?

IME, the most accurate possible measures of temp are required to get the highest resolution of fractionation/isolation possible. It is always recommended to use a thermometer which is designed and calibrated for lab purposes, that is contained inside the vacuum distillation environment, rather than measuring outside of the glass.

This is one hell of a debut post man! Your posts here comprise one of the greatest first contributions on this site! I'm beyond happy to see more people like yourself coming here, that are interested in advanced extractions/isolates! A very warm welcome to you once again!

One more question - do you retain the terpene fractions from these distillation runs? What do you do with that remaining material? :biggrin:
 
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EugeneOregon

New Member
I hope the information finds a good home. Thank you for providing this site for the general public. It is a real service needed in these times as we come out of an oppressive prohibition that forbid the research and passing along of knowledge and labelled it criminal.

Once upon a time a man also commited a crime by believing that the world was not flat and making any efforts to discover or report the truth were punishable by death. Burn the witch!!!

Thanks guys. Semper Fi
 

herbivore21

Well-Known Member
I hope the information finds a good home. Thank you for providing this site for the general public. It is a real service needed in these times as we come out of an oppressive prohibition that forbid the research and passing along of knowledge and labelled it criminal.

Once upon a time a man also commited a crime by believing that the world was not flat and making any efforts to discover or report the truth were punishable by death. Burn the witch!!!

Thanks guys. Semper Fi
Thank you for being here sir, I hope that you will continue to contribute! Yours here is the only time I've ever seen video footage of cannabis chromatography on such a site. You have done a great deal to reveal the inner workings of the science of separating cannabis resin into its constituent parts for all who visit here and that is commendable! :peace:
 

Baron23

Well-Known Member
@EugeneOregon and @herbivore21 - well, I'm glad to see you guys playing nicely and sharing toys! JK LOL

So, to you two the videos explain a lot. But to the less initiated, I have a hard time understanding Eugene's distillation rig (sorry Eugene, but as a movie director you are no Marty Scorsese) and it wasn't clear to me how exactly in this rig different compounds are separated.

Now, as pointed out....this really isn't tech for average home use....but I am interested. Not giving anyone homework, but perhaps a diagram and some explanation may be easier to digest than vids of your rig in action.

Or maybe I'm just bit dumb today! LOL

Cheers and a warm welcome, Eugene.
 

herbivore21

Well-Known Member
Now, as pointed out....this really isn't tech for average home use....but I am interested. Not giving anyone homework, but perhaps a diagram and some explanation may be easier to digest than vids of your rig in action.
A diagram with all components clearly labelled and list of components used would be wonderful, maybe @EugeneOregon can let us know of this information if he gets a chance. However, I am conscious that setting up, filming, managing all of that equipment etc is a lot of work for one person to do at once. The above would no doubt have been a hell of a lot more work to put together on one's own than your typical youtube rosin press video demonstration etc lol

@EugeneOregon and @herbivore21 - well, I'm glad to see you guys playing nicely and sharing toys! JK LOL
Man somebody with this rarer kind of advanced cannabis extraction knowledge like @EugeneOregon coming here is a wonderful, wonderful thing. I hope that we can have many more such contributors in the future! :biggrin:

I might start by explaining that actually, the videos above show two different methods. There is the distillation video, but also liquid chromatography.

Fractional distillation and chromatography are analytical methods, which could broadly be described as fundamental methods in the science of separation. These methods for cannabis will allow us to separate the various individual compounds within cannabis resin.

Fractional distillation, when it comes to cannabis, is what it sounds like. We can separately boil off various compounds of differing molecular weights by taking advantage of their different boiling points to separate the constituents within the resin. This can be used to separate THC/CBD/terpene fractions etc. The heat involved means that you're not going to get acidic compounds isolated using this method. Your THCA is going to become THC if you're distilling it.

If you wanna get acidic cannabinoids isolated, you could instead use Chromatography (typically liquid chromatography). Chromatography does have its own downsides, requiring what can be expensive and unusual solvents to source - yet another of many reasons for this not to be done at home by the uninitiated :dog:

Basically, in liquid chromatography (which Eugene used above), we pack a column with silica or alumina beads as @EugeneOregon did in his video above, then we devise an appropriate eluent (usually a mixture of two solvents, of differing polarity - Eugene used a mixture of Hexane and Ethyl Acetate, also some methanol. I have also heard of Hexane + Acetone mixtures being used with success here!). The appropriate eluent will vary depending on the analyte (substance you are trying to separate into constituents), the choice of solid phase (aka the 'adsorbent', ie: silica or alumina beads etc). There many be a variety of useful eluent solvents/co-solvent mixtures which will be appropriate here.

When the analyte is placed on top of the adsorbent beads in the column and then the eluent (solvent/s) is added, the analyte (resin in this case) dissolves into the solvents, and due to the properties of the solvent, different compounds start to descend down the column of adsorbent material at different speeds. The different chemicals are visibly observable by their different colors, so it is quite beautiful to watch this process in action - I encourage you to watch the respective video above.

At the bottom of the column is a stopcock, basically a place to drain the different colored fractions of 'eluate' (this describes the eluent, aka solvent/s containing a dissolved fraction isolated from the original resin) separately into different test tubes as they individually reach the bottom of the column.

It is important to have sufficiently slow elution speed (the speed that the different colored fractions descend down the column) to facilitate effective manual collection of each different sample that has been separated in the process into separate containers. This entails placing another collection vessel (usually a test tube, many of which would be prepared in racks for this purpose) below the column quickly to separately collect the different colored fractions as they come out through the stopcock.

A vacuum is used sometimes to facilitate the elution process in liquid chromatography, this is called High Performance Liquid Chromatography. When one uses no vacuum pressure, instead letting gravity do the work of separating the individual compounds within a crude extract as they elute, this is simply called 'Liquid Chromatography'.

I hope that this brief explanation of the two processes helps you guys understand what you see here for a start :peace:
 
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Baron23

Well-Known Member
A diagram with all components clearly labelled and list of components used would be wonderful, maybe @EugeneOregon can let us know of this information if he gets a chance. However, I am conscious that setting up, filming, managing all of that equipment etc is a lot of work for one person to do at once. The above would no doubt have been a hell of a lot more work to put together on one's own than your typical youtube rosin press video demonstration etc lol


Man somebody with this rarer kind of advanced cannabis extraction knowledge like @EugeneOregon coming here is a wonderful, wonderful thing. I hope that we can have many more such contributors in the future! :biggrin:

I might start by explaining that actually, the videos above show two different methods. There is the distillation video, but also liquid chromatography.

Fractional distillation and chromatography are analytical methods, which could broadly be described as fundamental methods in the science of separation. These methods for cannabis will allow us to separate the various individual compounds within cannabis resin.

Fractional distillation, when it comes to cannabis, is what it sounds like. We can separately boil off various compounds of differing molecular weights by taking advantage of their different boiling points to separate the constituents within the resin. This can be used to separate THC/CBD/terpene fractions etc. The heat involved means that you're not going to get acidic compounds isolated using this method. Your THCA is going to become THC if you're distilling it.

If you wanna get acidic cannabinoids isolated, you could instead use Chromatography (typically liquid chromatography). Chromatography does have its own downsides, requiring what can be expensive and unusual solvents to source - yet another of many reasons for this not to be done at home by the uninitiated :dog:

Basically, in liquid chromatography (which Eugene used above), we pack a column with silica or alumina beads as @EugeneOregon did in his video above, then we devise an appropriate eluent (usually a mixture of two solvents, of differing polarity - Eugene used a mixture of Hexane and Ethyl Acetate, also some methanol. I have also heard of Hexane + Acetone mixtures being used with success here!). The appropriate eluent will vary depending on the analyte (substance you are trying to separate into constituents), the choice of solid phase (aka the 'adsorbent', ie: silica or alumina beads etc). There many be a variety of useful eluent solvents/co-solvent mixtures which will be appropriate here.

When the analyte is placed on top of the adsorbent beads in the column and then the eluent (solvent/s) is added, the analyte (resin in this case) dissolves into the solvents, and due to the properties of the solvent, different compounds start to descend down the column of adsorbent material at different speeds. The different chemicals are visibly observable by their different colors, so it is quite beautiful to watch this process in action - I encourage you to watch the respective video above.

At the bottom of the column is a stopcock, basically a place to drain the different colored fractions of 'eluate' (this describes the eluent, aka solvent/s containing a dissolved fraction isolated from the original resin) separately into different test tubes as they individually reach the bottom of the column.

It is important to have sufficiently slow elution speed (the speed that the different colored fractions descend down the column) to facilitate effective manual collection of each different sample that has been separated in the process into separate containers. This entails placing another collection vessel (usually a test tube, many of which would be prepared in racks for this purpose) below the column quickly to separately collect the different colored fractions as they come out through the stopcock.

A vacuum is used sometimes to facilitate the elution process in liquid chromatography, this is called High Performance Liquid Chromatography. When one uses no vacuum pressure, instead letting gravity do the work of separating the individual compounds within a crude extract as they elute, this is simply called 'Liquid Chromatography'.

I hope that this brief explanation of the two processes helps you guys understand what you see here for a start :peace:

Thank you so very much. Very cogent and clear.

Couple of questions, if I may:

1. I understand fractional distillation in principle (like the cracking towers at oil refineries...yeah?) but its all dependent on their being a sufficient spread of boiling points of the various compounds, and sufficient precision/accuracy of temp controls, such that one can accurately and fully separate them one from another. What kind of temperature precision and accuracy is needed to do this with cannabis? Any idea?

2. I had no prior knowledge of liquid chromatography and my only exposure to that term was in reference to gas chromatography where the substance to be analyzed is heated to a gas and you can see the radiated spectrum of the different elements in the compound (and I'm 64 and this was in college so please take my understanding with a grain of salt). This is different and I appreciate the explanation. My question: how do you separate the different fractions if they are not indeed different colors. I get the drain it off from the bottom, layer by layer, but how well does this separate different molecules and how can you tell if they are not different colors (ok, probably a stupid question but I'm feeling particularly dense today haha).

Thanks
 

herbivore21

Well-Known Member
1. I understand fractional distillation in principle (like the cracking towers at oil refineries...yeah?) but its all dependent on their being a sufficient spread of boiling points of the various compounds, and sufficient precision/accuracy of temp controls, such that one can accurately and fully separate them one from another.
This is true, and so we need analytical testing after using processes like fractional distillation to confirm what we've separated from the original crude extraction. With some repeated practice and a robust database of repeatable (known as 'reliable' in scientific speak) results, the distiller can be more confident of the methods they will need to use to achieve the requisite separation that they are looking for.

What kind of temperature precision and accuracy is needed to do this with cannabis? Any idea?
As a general rule, as much precision of temp measurement and vacuum measurement as possible will assist in achieving repeatable results, especially in different labs with different equipment. Of course, even with a serviceable and safe ghetto setup that a sufficiently clever individual had cobbled together themselves (ATTENTION ALL READERS: DO NOT TRY THIS, PLEASE!), one could repeatedly do test runs and if the results showed consistent separations in analytical testing of the finished products, could achieve reliable fractional distillation of the required compounds without perfect measures.

Still, I would always advocate the most precise measurements possible of all key variables in any chemical process. Proper calibration of all relevant measurement tools is also important.

One problem for distillation is that some dangerous contaminants can have the same or similar molecular weights to target molecules (I have heard of THC and some pesticides sharing similar such properties which can be a real problem for fractional distillation of THC)!

I had no prior knowledge of liquid chromatography and my only exposure to that term was in reference to gas chromatography where the substance to be analyzed is heated to a gas and you can see the radiated spectrum of the different elements in the compound (and I'm 64 and this was in college so please take my understanding with a grain of salt).
Gas chromatography is also used in cannabis analytics, but of course the heat used means that you're gonna have trouble getting acidic cannabinoids like with fractional distillation.

Certainly not a completely outdated method my friend!

This is different and I appreciate the explanation. My question: how do you separate the different fractions if they are not indeed different colors. I get the drain it off from the bottom, layer by layer, but how well does this separate different molecules and how can you tell if they are not different colors (ok, probably a stupid question but I'm feeling particularly dense today haha).
If you do not get sufficient separation of substances with a given eluent, you might consider changes to the eluent and/or stationary phase which are more conducive to better, fuller and clearer separation of fractions. To confirm adequate separation, analytical testing results will still be required as above.

The degree of precision achieved is really going to depend not only on the eluent/adsorbent being used, but also the content of the resin being separated to begin with, and the extent to which sufficient analytical testing has been performed to confirm that the required compound/s have been isolated.

Over time and with experience, one may get used to how a particular fraction will look during chromatography of a specific substance using a specific solid phase and eluent. This may even allow a skilled and experienced chemist to adequately isolate target compounds without testing the results every single time.

I am sure that you can imagine just how expensive some of these processes could become, and how much crude extract one might require depending on what one is trying to isolate and how much they desire! Imagine the weight of extract required to isolate certain minor cannabinoids and terps!

I am sure that @EugeneOregon will have more specific responses to your questions based on his own experience with his own equipment and extracts too! I will not provide any actual figures since I've never done anywhere near enough chromatography/fractional distillation to generate reliable results from which to derive data that I could provide here.

I am so glad that we have this thread here now, since even if folks shouldn't try this at home, I think that patients and adult users all can benefit from understanding the nuts and bolts of these methods. It will allow for customers to ask the right questions and more easily understand the products that they purchase and in some cases, also allow customers to understand why some processes may lead to more expensive end products than others! :biggrin:
 

Baron23

Well-Known Member
Thank you so much for your reply. :thumbsup::clap::biggrin:

One problem for distillation is that some dangerous contaminants can have the same or similar molecular weights to target molecules (I have heard of THC and some pesticides sharing similar such properties which can be a real problem for fractional distillation of THC)!

Yes, this is what I was kind of going after.

I think that patients and adult users all can benefit from understanding the nuts and bolts of these methods. It will allow for customers to ask the right questions and more easily understand the products that they purchase and in some cases, also allow customers to understand why some processes may lead to more expensive end products than others! :biggrin:

Amen, brother!

Thanks again for taking the time to reply, my friend. I have absolutely no intention of trying either of these techniques myself, but gaining further understanding and knowledge never are a waste of time.

Cheers
 

EugeneOregon

New Member
A diagram with all components clearly labelled and list of components used would be wonderful, maybe @EugeneOregon can let us know of this information if he gets a chance. However, I am conscious that setting up, filming, managing all of that equipment etc is a lot of work for one person to do at once. The above would no doubt have been a hell of a lot more work to put together on one's own than your typical youtube rosin press video demonstration etc lol


Man somebody with this rarer kind of advanced cannabis extraction knowledge like @EugeneOregon coming here is a wonderful, wonderful thing. I hope that we can have many more such contributors in the future! :biggrin:

I might start by explaining that actually, the videos above show two different methods. There is the distillation video, but also liquid chromatography.

Fractional distillation and chromatography are analytical methods, which could broadly be described as fundamental methods in the science of separation. These methods for cannabis will allow us to separate the various individual compounds within cannabis resin.

Fractional distillation, when it comes to cannabis, is what it sounds like. We can separately boil off various compounds of differing molecular weights by taking advantage of their different boiling points to separate the constituents within the resin. This can be used to separate THC/CBD/terpene fractions etc. The heat involved means that you're not going to get acidic compounds isolated using this method. Your THCA is going to become THC if you're distilling it.

If you wanna get acidic cannabinoids isolated, you could instead use Chromatography (typically liquid chromatography). Chromatography does have its own downsides, requiring what can be expensive and unusual solvents to source - yet another of many reasons for this not to be done at home by the uninitiated :dog:

Basically, in liquid chromatography (which Eugene used above), we pack a column with silica or alumina beads as @EugeneOregon did in his video above, then we devise an appropriate eluent (usually a mixture of two solvents, of differing polarity - Eugene used a mixture of Hexane and Ethyl Acetate, also some methanol. I have also heard of Hexane + Acetone mixtures being used with success here!). The appropriate eluent will vary depending on the analyte (substance you are trying to separate into constituents), the choice of solid phase (aka the 'adsorbent', ie: silica or alumina beads etc). There many be a variety of useful eluent solvents/co-solvent mixtures which will be appropriate here.

When the analyte is placed on top of the adsorbent beads in the column and then the eluent (solvent/s) is added, the analyte (resin in this case) dissolves into the solvents, and due to the properties of the solvent, different compounds start to descend down the column of adsorbent material at different speeds. The different chemicals are visibly observable by their different colors, so it is quite beautiful to watch this process in action - I encourage you to watch the respective video above.

At the bottom of the column is a stopcock, basically a place to drain the different colored fractions of 'eluate' (this describes the eluent, aka solvent/s containing a dissolved fraction isolated from the original resin) separately into different test tubes as they individually reach the bottom of the column.

It is important to have sufficiently slow elution speed (the speed that the different colored fractions descend down the column) to facilitate effective manual collection of each different sample that has been separated in the process into separate containers. This entails placing another collection vessel (usually a test tube, many of which would be prepared in racks for this purpose) below the column quickly to separately collect the different colored fractions as they come out through the stopcock.

A vacuum is used sometimes to facilitate the elution process in liquid chromatography, this is called High Performance Liquid Chromatography. When one uses no vacuum pressure, instead letting gravity do the work of separating the individual compounds within a crude extract as they elute, this is simply called 'Liquid Chromatography'.

I hope that this brief explanation of the two processes helps you guys understand what you see here for a start :peace:

I chuckled when I read your comment about acetone being used. I purchase cheap grades mostly of solvents and the white and red can of Acetone is identical to the white and red can of Ethyl Acetate I get from Amazon. During an early experiment I was pretty stoned and trust me that Dry Column Vacuum Chromatography (DCVC) style Chromatography keeps even an organized person very busy during the run because the solvent gradient ration is constantly changing. Sooooooo..... you guessed it! I inadvertantly grabbed the Acetone can during the run and began using the acetone without realizing it in place of the EA. Oops.

If you look on the polarity charts which is roughly a gauge of the strength of solvents on any given stationary phase like silica gel, you will see that EA and Acetone are pretty close. My results were pretty close to what I might expect with EA but based on what I did observe during the botched experiment I do not plan to try that solvent system again. I have learned not to have both containers available in reach when only one is needed. I still plan to get high when I experiment though, so it is unclear if learning occured lolz.

Thank you so very much. Very cogent and clear.

Couple of questions, if I may:

1. I understand fractional distillation in principle (like the cracking towers at oil refineries...yeah?) but its all dependent on their being a sufficient spread of boiling points of the various compounds, and sufficient precision/accuracy of temp controls, such that one can accurately and fully separate them one from another. What kind of temperature precision and accuracy is needed to do this with cannabis? Any idea?

2. I had no prior knowledge of liquid chromatography and my only exposure to that term was in reference to gas chromatography where the substance to be analyzed is heated to a gas and you can see the radiated spectrum of the different elements in the compound (and I'm 64 and this was in college so please take my understanding with a grain of salt). This is different and I appreciate the explanation. My question: how do you separate the different fractions if they are not indeed different colors. I get the drain it off from the bottom, layer by layer, but how well does this separate different molecules and how can you tell if they are not different colors (ok, probably a stupid question but I'm feeling particularly dense today haha).

Thanks

Generally speaking (not always) in the chromatography runs I do, rather than trying to guess when to switch to the next fraction based on color, the fractions are collected in small samples one at a time and identified later. For instance, in the run I posted in the video I cannot target the acid form of THC versus the decarboxlylated form Delta 9 THC specifically. However I can isolate them by collecting small fractions in order and later identify it by allowing all the fraction to evaporate and sit out out room temps for a day or two. When I come back all but one or two fractions colllected will be mostly evaporated into a thick bubble free consistency with various colors. Many compounds like chlorophyl are easy to identify by color. Some are clear to the human eye or have colors so close the human eye cannot differentiate. THC and THCA are to close to tell apart by color.

The one or two fractions which elute from the column several fractions into the run that are different are different because they will be the consistency of swiss cheese instead of clear. There will be a lot of bubbles in the otherwise thick viscous compound which is generally in the fraction after the fractions with the orangest color which I believe to be carotanoids (What's up doc?). I can only deduce that that bubbles are representative from THCA decarboxylating into THC Delta 9. It sure seems like vaping that fraction after solvent purge has more "bite" to it to me. My lungs provide a sensitive measurment of the extract that labs cannot provide - direct observation and experience by using the product myself as medicine.

So you can see that it is the post run procedures that really identify what you are getting and when. How do we stop overlap of samples? We don't. As in distillation you only appraoch a point of better purity towards a target compound not perfect, and each runs produces progressively better purity if the protocol is sound. A lab instrument called a spectrophotometer that can identify ultraviolet absorbtion down to the 200 nm wavelength with a decent resolution can be employed to detect THC directly as well as most other constituents of the extract but the strategy is still to collect one small sample at a time then combine the like samples together.

I deny accusations that the drips of human drool on my ipad are from when I went online to look at spectophotometers on Amazon though....mostly....lolz

@EugeneOregon and @herbivore21 - well, I'm glad to see you guys playing nicely and sharing toys! JK LOL

So, to you two the videos explain a lot. But to the less initiated, I have a hard time understanding Eugene's distillation rig (sorry Eugene, but as a movie director you are no Marty Scorsese) and it wasn't clear to me how exactly in this rig different compounds are separated.

Now, as pointed out....this really isn't tech for average home use....but I am interested. Not giving anyone homework, but perhaps a diagram and some explanation may be easier to digest than vids of your rig in action.

Or maybe I'm just bit dumb today! LOL

Cheers and a warm welcome, Eugene.

Very kind! I have personally met the Hollywierd director types and trust me when I tell you without reservation that it is a deep compliment to me to be excluded from that group. Thank you hehe!

Distillation of any kind simply involves changing the phase of a material from liquid to gas and then recondensing the gas back into the liquid phase. In normal simple distillation what happens is that as vapor forms from the change in phases to a gas, the gas expands outward and upward and it flows much like any fluid might flow in a pipe. The "pipe" which carries the gas is called the uptake tube and it is then routed to a point in the apparatus to recondense in the receiver. Molecular distillation as I practice it on the face of it looks the same as simple distillation however there are real differences.

Molecular distillation as I use the phrase begins to occur somewhere below 100 microns as far as I know. When the vacuum is sufficiently deep the atoms no longer push off on one another when they are in the gas phase. My hunch is that the atoms are spread to thinly in deep vaccum to exert any force on each other without direct contact.

At any rate, once molecular distillation begins the liquid molecule changes phase into a gas, which then according to Brownian motion laws begins to travel in a random straight line direction under deep vacuum until it hits something cool enough for a phase transition back to liquid. So the molecules spread out and travel in a straight line path and while most end up right back in the flask, enough travel toward the boiling flask vessel exit that they progressively travel up the flask as a film and will continue to do so as long as the energy is applied to effect the phase change as described. The collection flask fills because once the molecules that move in random directions happen to move out of the boiling flask and into the much cooler receiving flask then they stop the process of repeatedly changing into gas and back to a liquid (phase changes) and remains liquid. The liquid then flows according to gravity and remains in the catch bulb.

THC has an extremely high boiling point at standard room pressures, so molecular distillation would normally be the best route if the goal is to distill at the lowest possible temperatures. Keep in mind that the vacuum pump itself is a participant here in molecular distillation. The oil used inside a pump capable of such deep vacuum can and does itself change phases into a gas and then recondense as I describe in a random straight line direction. This means that even though the process is very slow with the pump oil that it does indeed travel up out of the pump and up the vacuum supply line until there is not enough energy present to keep the cycle going like when the pump is off.

Traps are available to slow this potential contamination. They are called "foreline traps" and work on the principle that because the oil travels in a straight line under molecular distillation, that a trap filled with inert alumina beads that the vacuum travels through presents the longest possible path with many interuptions to a straight line as possible for the vacuum pump oil to "creep" though in this manner and up the vacuum supply line.

The process is not overly complicated though the explanation might seem so. The process is much easier to run than my sewing machine really, but a complete understanding of the process helps visualization of the possibilities better. A two neck flask with a thermometer is my next purchase and I already have the adapter and thermometer. With this I hope to measure the liquid and the vapor temperatures directly while under molecular distillation. Like a model train set, it just seems that there is one more piece I always still need...

Mod note: Three posts merged.
 
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herbivore21

Well-Known Member
I chuckled when I read your comment about acetone being used. I purchase cheap grades mostly of solvents and the white and red can of Acetone is identical to the white and red can of Ethyl Acetate I get from Amazon. During an early experiment I was pretty stoned and trust me that Dry Column Vacuum Chromatography (DCVC) style Chromatography keeps even an organized person very busy during the run because the solvent gradient ration is constantly changing. Sooooooo..... you guessed it! I inadvertantly grabbed the Acetone can during the run and began using the acetone without realizing it in place of the EA. Oops.
Oh man, fortunate that it wasn't a solvent that was much less fit for the task at hand! I myself have had one or two missteps where reaching for the wrong solvent cost me a whole lot more than I care to think about :dog:

If you look on the polarity charts which is roughly a gauge of the strength of solvents on any given stationary phase like silica gel, you will see that EA and Acetone are pretty close.
Indeed, what I love about chromatography is that there isn't just one way to get the required separation. I've heard of all kinds of combinations being used, especially when you start to look at the scholarly literature on analytical isolation of THC and related compounds for use in drug testing.

My results were pretty close to what I might expect with EA but based on what I did observe during the botched experiment I do not plan to try that solvent system again. I have learned not to have both containers available in reach when only one is needed. I still plan to get high when I experiment though, so it is unclear if learning occured lolz.
What was the difference in end result that you observed in this case? I'm fascinated to hear your observations man, it is such a pleasure to have you here! Are there any other potential causal variables that you ruled out first?

Also you and I are in lock step on doing experiments while medicated. For me, due to my own disabilities, I actually make less negligent/careless mistakes like reaching for the wrong solvent when I am medicated with cannabis. What a wonderful plant we have here, I'm sure you agree my friend! :weed:

Generally speaking (not always) in the chromatography runs I do, rather than trying to guess when to switch to the next fraction based on color, the fractions are collected in small samples one at a time and identified later. For instance, in the run I posted in the video I cannot target the acid form of THC versus the decarboxlylated form Delta 9 THC specifically. However I can isolate them by collecting small fractions in order and later identify it by allowing all the fraction to evaporate and sit out out room temps for a day or two. When I come back all but one or two fractions colllected will be mostly evaporated into a thick bubble free consistency with various colors. Many compounds like chlorophyl are easy to identify by color. Some are clear to the human eye or have colors so close the human eye cannot differentiate. THC and THCA are to close to tell apart by color.
Have you considered crystallization as a step towards isolating THCA? Or are specifically looking for delta 9 THC for your purposes?

Very kind! I have personally met the Hollywierd director types and trust me when I tell you without reservation that it is a deep compliment to me to be excluded from that group. Thank you hehe!
:dog:

Traps are available to slow this potential contamination. They are called "foreline traps" and work on the principle that because the oil travels in a straight line under molecular distillation, that a trap filled with inert alumina beads that the vacuum travels through presents the longest possible path with many interuptions to a straight line as possible for the vacuum pump oil to "creep" though in this manner and up the vacuum supply line.
Indeed, additionally as I mentioned above (and as I'm sure you knew already), oil-less vacuum pumps are also available that are designed to avoid this issue in the first place - for an additional cost.

A two neck flask with a thermometer is my next purchase and I already have the adapter and thermometer. With this I hope to measure the liquid and the vapor temperatures directly while under molecular distillation. Like a model train set, it just seems that there is one more piece I always still need...
I look forward to hearing of your results and findings with the thermometer inside the system rather than around the glass! I'd love to pick your brain and send you a PM one day when the time comes and I get some time for a few experiments of my own, if you'd be willing!

Can I ever relate to you on that model train set analogy by the way - there's always another must-have piece of extraction equipment on the horizon isn't there!? :dog:

This thread has already done an enormous amount of good in demystifying distillation (I'm sure there's a pun in there!) for readers - again, thank you and the warmest of welcomes to you, it has already been a privilege!
 

EugeneOregon

New Member
I chuckled when I read your comment about acetone being used. I purchase cheap grades mostly of solvents and the white and red can of Acetone is identical to the white and red can of Ethyl Acetate I get from Amazon. During an early experiment I was pretty stoned and trust me that Dry Column Vacuum Chromatography (DCVC) style Chromatography keeps even an organized person very busy during the run because the solvent gradient ration is constantly changing. Sooooooo..... you guessed it! I inadvertantly grabbed the Acetone can during the run and began using the acetone without realizing it in place of the EA. Oops.

If you look on the polarity charts which is roughly a gauge of the strength of solvents on any given stationary phase like silica gel, you will see that EA and Acetone are pretty close. My results were pretty close to what I might expect with EA but based on what I did observe during the botched experiment I do not plan to try that solvent system again. I have learned not to have both containers available in reach when only one is needed. I still plan to get high when I experiment though, so it is unclear if learning occured lolz.



Generally speaking (not always) in the chromatography runs I do, rather than trying to guess when to switch to the next fraction based on color, the fractions are collected in small samples one at a time and identified later. For instance, in the run I posted in the video I cannot target the acid form of THC versus the decarboxlylated form Delta 9 THC specifically. However I can isolate them by collecting small fractions in order and later identify it by allowing all the fraction to evaporate and sit out out room temps for a day or two. When I come back all but one or two fractions colllected will be mostly evaporated into a thick bubble free consistency with various colors. Many compounds like chlorophyl are easy to identify by color. Some are clear to the human eye or have colors so close the human eye cannot differentiate. THC and THCA are to close to tell apart by color.

The one or two fractions which elute from the column several fractions into the run that are different are different because they will be the consistency of swiss cheese instead of clear. There will be a lot of bubbles in the otherwise thick viscous compound which is generally in the fraction after the fractions with the orangest color which I believe to be carotanoids (What's up doc?). I can only deduce that that bubbles are representative from THCA decarboxylating into THC Delta 9. It sure seems like vaping that fraction after solvent purge has more "bite" to it to me. My lungs provide a sensitive measurment of the extract that labs cannot provide - direct observation and experience by using the product myself as medicine.

So you can see that it is the post run procedures that really identify what you are getting and when. How do we stop overlap of samples? We don't. As in distillation you only appraoch a point of better purity towards a target compound not perfect, and each runs produces progressively better purity if the protocol is sound. A lab instrument called a spectrophotometer that can identify ultraviolet absorbtion down to the 200 nm wavelength with a decent resolution can be employed to detect THC directly as well as most other constituents of the extract but the strategy is still to collect one small sample at a time then combine the like samples together.

I deny accusations that the drips of human drool on my ipad are from when I went online to look at spectophotometers on Amazon though....mostly....lolz



Very kind! I have personally met the Hollywierd director types and trust me when I tell you without reservation that it is a deep compliment to me to be excluded from that group. Thank you hehe!

Distillation of any kind simply involves changing the phase of a material from liquid to gas and then recondensing the gas back into the liquid phase. In normal simple distillation what happens is that as vapor forms from the change in phases to a gas, the gas expands outward and upward and it flows much like any fluid might flow in a pipe. The "pipe" which carries the gas is called the uptake tube and it is then routed to a point in the apparatus to recondense in the receiver. Molecular distillation as I practice it on the face of it looks the same as simple distillation however there are real differences.

Molecular distillation as I use the phrase begins to occur somewhere below 100 microns as far as I know. When the vacuum is sufficiently deep the atoms no longer push off on one another when they are in the gas phase. My hunch is that the atoms are spread to thinly in deep vaccum to exert any force on each other without direct contact.

At any rate, once molecular distillation begins the liquid molecule changes phase into a gas, which then according to Brownian motion laws begins to travel in a random straight line direction under deep vacuum until it hits something cool enough for a phase transition back to liquid. So the molecules spread out and travel in a straight line path and while most end up right back in the flask, enough travel toward the boiling flask vessel exit that they progressively travel up the flask as a film and will continue to do so as long as the energy is applied to effect the phase change as described. The collection flask fills because once the molecules that move in random directions happen to move out of the boiling flask and into the much cooler receiving flask then they stop the process of repeatedly changing into gas and back to a liquid (phase changes) and remains liquid. The liquid then flows according to gravity and remains in the catch bulb.

THC has an extremely high boiling point at standard room pressures, so molecular distillation would normally be the best route if the goal is to distill at the lowest possible temperatures. Keep in mind that the vacuum pump itself is a participant here in molecular distillation. The oil used inside a pump capable of such deep vacuum can and does itself change phases into a gas and then recondense as I describe in a random straight line direction. This means that even though the process is very slow with the pump oil that it does indeed travel up out of the pump and up the vacuum supply line until there is not enough energy present to keep the cycle going like when the pump is off.

Traps are available to slow this potential contamination. They are called "foreline traps" and work on the principle that because the oil travels in a straight line under molecular distillation, that a trap filled with inert alumina beads that the vacuum travels through presents the longest possible path with many interuptions to a straight line as possible for the vacuum pump oil to "creep" though in this manner and up the vacuum supply line.

The process is not overly complicated though the explanation might seem so. The process is much easier to run than my sewing machine really, but a complete understanding of the process helps visualization of the possibilities better. A two neck flask with a thermometer is my next purchase and I already have the adapter and thermometer. With this I hope to measure the liquid and the vapor temperatures directly while under molecular distillation. Like a model train set, it just seems that there is one more piece I always still need...

Mod note: Three posts merged.
Here is a shut down video while the unit is still distilling over but afger heat removed. Vacuum pump still on, and this one shows the unit much better to get an idea of the simple concept works.
 

EugeneOregon

New Member
I just vaped some of the "test" compound collected during this selfless scientific experiment only because the subject matter requires a "subjective" evaluation (my protocol specifies this) or the whole experiment is shot! I am willing to make this sacrifice for science though.... We all have to do our part....:smug:

On a scale of one to ten the potency scores a "yes". Somehow at this moment that makes perfect sense to me although I suspect that when I get back to Earth that things will change. enjoy!

 

herbivore21

Well-Known Member
I just vaped some of the "test" compound collected during this selfless scientific experiment only because the subject matter requires a "subjective" evaluation (my protocol specifies this) or the whole experiment is shot! I am willing to make this sacrifice for science though.... We all have to do our part....:smug:

On a scale of one to ten the potency scores a "yes". Somehow at this moment that makes perfect sense to me although I suspect that when I get back to Earth that things will change. enjoy!

Thanks for sharing and great to see you got your new thermometer piece :biggrin::science:

Out of interest, have you ever had analytical testing carried out on your fractions? I'd be very interested (as I'm sure you would!) to learn exactly what degree of isolation you're getting!

What is your starting material in the pot there by the way? Do you start with an ethanol extract and then distill?
 

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