[EugeneOregon]

Idles hands early early in the morning are up to the Devil's business; Art!!! The question is what to call it? Is this "Pure Art" (PA) or "Dabable Craftsmanship" (DC). I a gonna take a dab then decide...

https://www.youtube.com/watch?v=KXhr...5jxy2pw03c010c

[mack 10]

Oops nearly drops it right at the start.
lol

[Badfishy1]

Originally Posted by EugeneOregon

Idles hands early early in the morning are up to the Devil's business; Art!!! The question is what to call it? Is this "Pure Art" (PA) or "Dabable Craftsmanship" (DC). I a gonna take a dab then decide...

https://www.youtube.com/watch?v=KXhr...5jxy2pw03c010c

Looking proper m8

[live resin]

Kinda sloppy on the DCVC in the other videos. You can see the channeling from not packing the edges of the column properly. And he should have dry loaded the column using Celite IMO. And while the fractions collected for use might be almost pure cannabinoids, they are surely not pure d9THC as claimed in the other videos. For 99%+ d9THC you'd probably have to do a final polishing step with gel chromatography

[EugeneOregon]

Originally Posted by live resin

Kinda sloppy on the DCVC in the other videos. You can see the channeling from not packing the edges of the column properly. And he should have dry loaded the column using Celite IMO. And while the fractions collected for use might be almost pure cannabinoids, they are surely not pure d9THC as claimed in the other videos. For 99%+ d9THC you'd probably have to do a final polishing step with gel chromatography

In my online video that displays banding, improper packing on the sides was only one problem. The second problem was that I wet loaded onto the silica gel 60 using extract that still contained methanol. This is what moved so much of the sample into the gel column initially which loaded up the gel on top in a messy way. The third problem was also a packing problem insofar as I only used the vacuum to pack it and have since learned to simultaneously pack it down with a large wood dowel. Sides are packed now with a small spatula I made.

I often employ dry loading with Celite however Celite has a drawback for me. I use chromatography as a preparatory process, not an analytical one. In order for Celte to work well it has to be totally dry after the compound is attached to the celite. THC and the rest of my extract components are very sticky so a lot of Celite is needed. I found that when doing more than just a few grams at a time that the volumn of celite needed to hold the volume of extract I wanted to run exceeded my quick seperation funnels capacity to hold it all. I even attempted loading celite in a funnel above the column in a funnel to hold it all once! What a disaster!!!

Celite is extremely nice for small samples and the seperation can be crisp and clean but will not work for the samples I sometimes run because of volume. What I have learned to do from those experiments is to avoid celite dry loading for anything over about three grams because my quick sep funnel cannot hold more in a single run. The run effectively becomes a wet loaded column when that much Celite is used. Second, my DCVC revealled that silica gel 60 does not pass cannabinoid or hardly anything at all in extract when it is disolved solely in hexane. So now I load the sample completely disolved in the mimimum amount of hexane that will disolve it and place it on top of the silica gel. The seperation will not begin until I add a half pipette of ethyl acetate to the sample. Then once the wet loaded sample is pulled into the column I proceed with the EA/Hexane gradient as planned.

You have a sharp eye and very good analytical observation!

There is no way from the videos to determine if any of the products shown are either pure or not pure except for color and it is rare and only under molecular distillation that I see a color I believe would approach pure thc. It presents itself as a very pale yellow jelly like substance at room temp and although the taste is vague it is sweet in flavor in the same fashion that cold water on a very hot day can taste sweet when you are parched. It is an aftertaste and it is pleasant. However, in the absence of qualitative testing via gas chromatography then the only testing possible that provides qualitative data is personal sampling and vaping.

Personal vaping of course does not produce a result that can be expressed as a percentage, so I break down the description into subjective phrases like, "very good", "excellent", "harsh", "Terpy", and "nearly pure" and whatever else comes into my stoned mind when I am holding an ipad in one hand to take vid while conducting an experiement. These are not claims at all - they are subjective descriptions. A posted number, like the one you posted is a claim and has no subjective evidence to support it. Subjective observations do not need validation with numbers as they only serve to in advisory roles. It is anecdotal information. There is no way anyone can determine numbers either high or low from a video obviously.

I have sampled each fraction after solvent purge from the multiple fractions produced (even the green ones) from chromatography. I call the green one the chlorophyl fraction but cannot confirm with numbers that it represents the bulk of the chlorophyl in the plant. However even without numbers to toss around I still believe that the green fraction is in fact chlorophyl and this too is a subjective observation.

The purpose of the videos is to present data. I look forward to seeing others present videos that can improve upon my the methods that I use and perhaps add numerical and more objective data for the community.

[Badfishy1]

Originally Posted by EugeneOregon

In my online video that displays banding, improper packing on the sides was only one problem. The second problem was that I wet loaded onto the silica gel 60 using extract that still contained methanol. This is what moved so much of the sample into the gel column initially which loaded up the gel on top in a messy way. The third problem was also a packing problem insofar as I only used the vacuum to pack it and have since learned to simultaneously pack it down with a large wood dowel. Sides are packed now with a small spatula I made.

I often employ dry loading with Celite however Celite has a drawback for me. I use chromatography as a preparatory process, not an analytical one. In order for Celte to work well it has to be totally dry after the compound is attached to the celite. THC and the rest of my extract components are very sticky so a lot of Celite is needed. I found that when doing more than just a few grams at a time that the volumn of celite needed to hold the volume of extract I wanted to run exceeded my quick seperation funnels capacity to hold it all. I even attempted loading celite in a funnel above the column in a funnel to hold it all once! What a disaster!!!

Celite is extremely nice for small samples and the seperation can be crisp and clean but will not work for the samples I sometimes run because of volume. What I have learned to do from those experiments is to avoid celite dry loading for anything over about three grams because my quick sep funnel cannot hold more in a single run. The run effectively becomes a wet loaded column when that much Celite is used. Second, my DCVC revealled that silica gel 60 does not pass cannabinoid or hardly anything at all in extract when it is disolved solely in hexane. So now I load the sample completely disolved in the mimimum amount of hexane that will disolve it and place it on top of the silica gel. The seperation will not begin until I add a half pipette of ethyl acetate to the sample. Then once the wet loaded sample is pulled into the column I proceed with the EA/Hexane gradient as planned.

You have a sharp eye and very good analytical observation!

There is no way from the videos to determine if any of the products shown are either pure or not pure except for color and it is rare and only under molecular distillation that I see a color I believe would approach pure thc. It presents itself as a very pale yellow jelly like substance at room temp and although the taste is vague it is sweet in flavor in the same fashion that cold water on a very hot day can taste sweet when you are parched. It is an aftertaste and it is pleasant. However, in the absence of qualitative testing via gas chromatography then the only testing possible that provides qualitative data is personal sampling and vaping.

Personal vaping of course does not produce a result that can be expressed as a percentage, so I break down the description into subjective phrases like, "very good", "excellent", "harsh", "Terpy", and "nearly pure" and whatever else comes into my stoned mind when I am holding an ipad in one hand to take vid while conducting an experiement. These are not claims at all - they are subjective descriptions. A posted number, like the one you posted is a claim and has no subjective evidence to support it. Subjective observations do not need validation with numbers as they only serve to in advisory roles. It is anecdotal information. There is no way anyone can determine numbers either high or low from a video obviously.

I have sampled each fraction after solvent purge from the multiple fractions produced (even the green ones) from chromatography. I call the green one the chlorophyl fraction but cannot confirm with numbers that it represents the bulk of the chlorophyl in the plant. However even without numbers to toss around I still believe that the green fraction is in fact chlorophyl and this too is a subjective observation.

The purpose of the videos is to present data. I look forward to seeing others present videos that can improve upon my the methods that I use and perhaps add numerical and more objective data for the community.

Pardon my ignorance, but what process to you use for the solvent purge?

[EugeneOregon]

Originally Posted by Badfishy1

Pardon my ignorance, but what process to you use for the solvent purge?

I have a chemical duty diaphragm pump constructed internally of PTFE (teflon). I generally allow the bulk of solvent to evaporate away at room temp as much as will evaporate. Then I place the extract into a small flask and pull a vacuum with my PTFE pump then heat the extract in the mantle to at least 250F.

Solvent recovery is easy but problematic because of water. Iso and ethanol form azeotropes with water as does acetone and ethyl acetate. Methanol will not form an azeotrope so it can indeed be purified by fractional distillation but the others cannot be distilled into purity owing to the azeotrope with water. So when I recover solvent it is really really only to recycle it as a cleaning agent because the purity is shit unless measure to purify it are undertaken and for an ounce or two it is not worth it to me. Generally anything miscible in water will also soak it up water from atmosphere and from the moment the container is opened the water begins getting in.

So I choose to pull a deep vacuum and purge it to atmosphere through a PTFE pump. I also have a small glass shattervac chamber that I use if the boilng flask is not convenient.

[Badfishy1]

Originally Posted by EugeneOregon

I have a chemical duty diaphragm pump constructed internally of PTFE (teflon). I generally allow the bulk of solvent to evaporate away at room temp as much as will evaporate. Then I place the extract into a small flask and pull a vacuum with my PTFE pump then heat the extract in the mantle to at least 250F.

Solvent recovery is easy but problematic because of water. Iso and ethanol form azeotropes with water as does acetone and ethyl acetate. Methanol will not form an azeotrope so it can indeed be purified by fractional distillation but the others cannot be distilled into purity owing to the azeotrope with water. So when I recover solvent it is really really only to recycle it as a cleaning agent because the purity is shit unless measure to purify it are undertaken and for an ounce or two it is not worth it to me. Generally anything miscible in water will also soak it up water from atmosphere and from the moment the container is opened the water begins getting in.

So I choose to pull a deep vacuum and purge it to atmosphere through a PTFE pump. I also have a small glass shattervac chamber that I use if the boilng flask is not convenient.

Damn still have lots to learn

[G.O. Joe]

Originally Posted by EugeneOregon

However, in the absence of qualitative testing via gas chromatography then the only testing possible that provides qualitative data is personal sampling and vaping.

TLC

If you really care, you have to remove the s that the board adds to http regardless.