First of all, let me say, that your videos are awesome. Now, I do not know your background but if already know this pass it, if not, her are some information. SFE occurs in different stages, first, the vegetal matrix absorbs the supercritical solvent, swelling its cellular structure, membranes and dilating the intercellular channels, leading to a drop in the resistance to mass transfer; in the meantime, dissolution of the extract occurs, and mass transfer take place from the inner matrix to its surface and solubilized compounds reach the external surface. These are finally transported from the surface to the supercritical solvent and removed from the solvent. So, this happens in various stages: 1- First there is a constant extraction rate period, where the external surface of the particles is covered with solute (easily accessible solute) and the convection (in the CO2) is the dominant mass transfer mechanism. 2- Secondly, there's a falling extraction rate where failures in the external surface oil layer appear and the diffusion mechanism starts, operating combined with convection; c) Lastly, there's a Low Extraction Rate or Diffusion-Controlled (DC) period, where the external layer of oil practically disappeared and the mass transfer occurs mainly by diffusion inside the solid particles. So, you're dependent on the biomass matrix itself, and you should grind the beans, increasing the surface area thus enabling a better impregnation of the biomass, increasing the solubilization of the target molecules and also insuring a better mass transfer from the biomass matrix to the CO2. In your case (maximum yield and lower extraction time possible) you should operate on the first to second phase. Oh and the extraction result isn't pure caffeine. Some tips: Water in the biomass increases the celular turgor and helps to increase the yield of the SFE by allowing a better impregnation of the biomass, but don't mistake it for cosolvent modifier, these are used to extract other type of molecules (hidrophilic/polar fraction) and these can also be used to manipulate selectivity of the extraction. Grinded coffee beans translates in increased yield. You could bubble the outlet of the extraction into an ethanol solution thus allowing better distillation afterwards. That bursts of CO2 you have on the outlet of the vessel when CO2 forms ice, blocking the pass, you could heat up that outlet zone with the electric heating mantle and that would decrease that. Cheers!
I totally agree. The approach he uses feels very counterintuitive, aswell as the soaking. If the h20 takes up the intracelluar matrix and dissolves the caffeine, wouldn't the co2 and h20 just compete with solubility?
This is just awesome! I have worked with supercritical drying for my bachelor's and master's work and I remember fondly the pain in the ass that is drying aerogels and extraction if caffeine that my colleagues ran. CO2 freezing in the valve was a major problem, if you still run it try just heating it with the heating tape or air gun...And again, you are awesome for making this happen in at home. Congrats on the great content!
This was a very cool expriment. I saw your first attempt a little while ago. I think the best part though is hearing the bit of giddiness in your voice as you talk about some of these things. More people need to have this kind of appreciation of science.
Excellent video and channel! I guess by now someone must have had this idea, but... I guess the black solute in the extract is either iron carbonate or iron oxide. Maybe the water from the beans reacted with the CO2 to form carbonic acid, which in turn reacted with the steel pipe. That would explain why only some of the beans are dark; it´s probably those that were touching the wall. At work we need to purge lines when refilling CO2 tanks so no air moisture gets inside the tank because if it does time over time, internal corrosion takes place.
you sir, are a genius. no kidding either, this is really impressive that someone would do thin in their garage! ill have to do this for science fair! excellent video too!
@Ammoniummetavanadate Sorry, it is grade 2, not grade 1. We do work with sulphides and chlorides, pure Ti is one of the only things that can reliably stand up to them.
Your video is great. Do you know is there any commercial scale supercritical co2 extraction plant working on decaffeination for green beans in the world currelty? Thank you
Good video, and work. May I suggest using redundant pressure relief safety valves (if its possible to have it to the correct pressure), a thicker viewing portal, and grinding up the coffee beans. Is aluminum a concern for leaching into the essential oil?
hey friend im shure you thought of this but have u considerd draning the co2 by using the valve on top first, to say 50 psi , imnot shure but i dont think dry ice will form at this pressure , then you coulddrain your most awsome coffee ever......
did the water become acidic via carbonic acid which cause the steel create the black residue? i seem to remember playing with acids and iron and it turning black, but for the life of me cant remember much more then that. ps, love your work
@bkraz333 that may be a bit dangerous it you end up with a extremely high percentage of pure caffeine. And how much did that shop cost to construct and what do you do for a living as i am hoping to go into the biology field?
I find this experiment and household application of chemistry and thermodynamics to be quite interesting. I was wondering if you have an estimate on how much this scale experiment costed, where you got liquid CO2 from, and what safety precautions you had to take? I would have been quite frightened to have the pressure exceed the the working pressure of the sight glass.
Supercritical fluid extraction can be more selective than other extraction means - but I would still expect it to extract all other free base alkaloids from the coffee beans as well. This might also change the taste of the decaffeinated beans beyond just the taste component given by caffeine - AND it also means your extracted caffeine is not 100% pure - I would still be very curious what purity grade that is (and whether or not it is high - like 80-100% or much lower). Do you know anything about that?
This has probably been mentioned but I imagine the black color was from the iron pipe you used and not the coffee beans. Have you considered using a stainless steel chamber, Though I imagine that might be a touch expensive.
FYI robusta coffee beans contain more caffeine than arabica beans. Btw you're set up is awesome. I've tried the crystallized caffeine, it has a rather nasty taste.
Tannins! I remember that iron (I think a mixture of Fe(2+) and Fe(3+) is required, or maybe it's just one, I forget) reacts with tannins to produce a dark bluish-blacky ink. Iron is acidic, and takes a reasonable acid to keep it in solution, so this type of ink, though easy to make, was quite destructive to paper. I'm willing to bet your supercritical espresso shot had more than your daily dose of iron in it as well!
Why does there need to be water in the system? Is the solubility of caffeine that low in supercritical CO2? I was expecting a pipe with beans that got half filled with liquid CO2, turn it supercritical and in order to extract the solid all you would need to do would be to evaporate the CO2 leaving you with a pile of caffeine. Can supercritical CO2 not dissolve a significant enough g/ml in them compared to water?
An aqueous iron solution will turn opaque and black if tea or coffee are introduced. As it happens, that's a method of making ink, though I first learned about it by playing with 2L pop bottles of iron-rich well water adding a single drop of tea to make the whole volume slowly change. I don't know enough about the reaction to say whether it contributed, but I figured I'd mention it for completeness.
No. Did you just make that up on the spot? From wikipedia: "Part of the reason caffeine is classified by the Food and Drug Administration as GRAS (generally recognized as safe) is that toxic doses (over 1 gram for an average adult) are much higher than typically used doses (less than 500 milligrams)."
With the pressure vessel you made from aluminium and acrylic, would the liquid CO2 leak out over large time scales? or is it reasonably stable? IE: could I make one and have a really cool workshop ornament?
You should know that Teflon tape does not seal the pipe, its purpose is to facilitate (as a dry lubricant) the screwing of the taper pipe threads, thus allowing for a better seal.
@sabamacx Well since he based the procedure off a patent it's a pretty safe bet. I'd imagine that the patent proved that the product was caffeine (i.e. through chemical analyses such as qualitative features, TLC, mass spectrometry, or NMR spectroscopy).
right on w your success!!! you must not over fill the vessels w plant matter. A plug can occur between the gauge and or valves and when you open this plugged vessel, the final threads will fail sending the top off like a cannon. the pressure difference of the blast is very lethal and anyone w in that radius is in danger. be careful and try employing safety relief valves for G.P.
Would this work for catnip? I have access to really cheap catnip, but I wonder if extracting it with CO2 would be possible. I'm considering running it in a ball mill to make a really fine powder before the extract, and then using some DCM might work to create a pure nepetalactone extract.
soooo.... ok ill ask, have you ever expertimented with more nefreious substances in that lab of yours... i mean... all these chemicals all this know how... have you ever made any illegal substances?
First of all, let me say, that your videos are awesome.
Now, I do not know your background but if already know this pass it, if not, her are some information.
SFE occurs in different stages, first, the vegetal matrix absorbs the supercritical solvent, swelling its cellular structure, membranes and dilating the intercellular channels, leading to a drop in the resistance to mass transfer; in the meantime, dissolution of the extract occurs, and mass transfer take place from the inner matrix to its surface and solubilized compounds reach the external surface. These are finally transported from the surface to the supercritical solvent and removed from the solvent.
So, this happens in various stages:
1- First there is a constant extraction rate period, where the external surface of the particles is covered with solute (easily accessible solute) and the convection (in the CO2) is the dominant mass transfer mechanism.
2- Secondly, there's a falling extraction rate where failures in the external surface oil
layer appear and the diffusion mechanism starts, operating combined with
convection;
c) Lastly, there's a Low Extraction Rate or Diffusion-Controlled (DC) period, where the
external layer of oil practically disappeared and the mass transfer occurs mainly
by diffusion inside the solid particles.
So, you're dependent on the biomass matrix itself, and you should grind the beans, increasing the surface area thus enabling a better impregnation of the biomass, increasing the solubilization of the target molecules and also insuring a better mass transfer from the biomass matrix to the CO2. In your case (maximum yield and lower extraction time possible) you should operate on the first to second phase.
Oh and the extraction result isn't pure caffeine.
Some tips:
Water in the biomass increases the celular turgor and helps to increase the yield of the SFE by allowing a better impregnation of the biomass, but don't mistake it for cosolvent modifier, these are used to extract other type of molecules (hidrophilic/polar fraction) and these can also be used to manipulate selectivity of the extraction.
Grinded coffee beans translates in increased yield.
You could bubble the outlet of the extraction into an ethanol solution thus allowing better distillation afterwards.
That bursts of CO2 you have on the outlet of the vessel when CO2 forms ice, blocking the pass, you could heat up that outlet zone with the electric heating mantle and that would decrease that.
Cheers!
Damn
I totally agree. The approach he uses feels very counterintuitive, aswell as the soaking. If the h20 takes up the intracelluar matrix and dissolves the caffeine, wouldn't the co2 and h20 just compete with solubility?
Yeah, I'm always floored by the work Ben does. This is incredibly interesting -- and I love the DIY angle.
This is just awesome! I have worked with supercritical drying for my bachelor's and master's work and I remember fondly the pain in the ass that is drying aerogels and extraction if caffeine that my colleagues ran. CO2 freezing in the valve was a major problem, if you still run it try just heating it with the heating tape or air gun...And again, you are awesome for making this happen in at home. Congrats on the great content!
Would be awesome if his voice sped up after 7:55 and the camera got super shakey.
It’s 2020 and I’m in quarantine. This channel is keeping me sane
Shane Ellis same
Ben you've got some fascinating videos. Kudos, the world needs more people like you.
Yeah but what happened when you snorted it?
+Will Whitez cocaine is what happened
It ain't easy being cheezy.
Wenk Hsueh
He went supercritical.
MPSecare Lars Ulrich
Love the detail you go into explaining the process, also how excited you sound at the beginning of the video.
This was a very cool expriment. I saw your first attempt a little while ago. I think the best part though is hearing the bit of giddiness in your voice as you talk about some of these things. More people need to have this kind of appreciation of science.
Your video are something so great to watch. I wan't to give big thanks from Finland to you for sharing all these with us TH-camr's !
Excellent video and channel!
I guess by now someone must have had this idea, but... I guess the black solute in the extract is either iron carbonate or iron oxide. Maybe the water from the beans reacted with the CO2 to form carbonic acid, which in turn reacted with the steel pipe. That would explain why only some of the beans are dark; it´s probably those that were touching the wall. At work we need to purge lines when refilling CO2 tanks so no air moisture gets inside the tank because if it does time over time, internal corrosion takes place.
4:29 "Time to get my GIANT PIPE WRENCH"
+urdnal oh wait it's a more or less normal pipe wrench with a pipe for leverage on it. I'm a little disappointed
+urdnal
I wouldn't have noticed the pipe if not for you.
That is a man confident in his work. Drinking that black liquid. Wow.
@bkraz333
you are probably the master of extracting thc from the herb.
You might be the coolest guy there is... a true renaissance man.
Appreciate your efforts to upload your experiments. Great stuff!
Just imagining people doing lines of purified caffeine
I am curious about that
it would probably give you a heart-attack
68.25mg x your weight = how much in mg will kill you
I am assuming the mas is in kilograms?
Alex Rhodes
so thats how all of your lightbulbs end up in the trash with big black spots all over ....
- Of course, I had to taste it
:D
Fantastic video again. You're batting 1000. Thanks so much for posting these.
Another inspirational example of personal industry.
You're a mad scientist, sir, and I salute you.
you sir, are a genius.
no kidding either, this is really impressive that someone would do thin in their garage! ill have to do this for science fair! excellent video too!
You are a crazy cool scientist^^ And the best i think is that u do it in your free time. Cool Hobby!
now you finished 2011 with a flourish! your new year's eve will have decaffeinated coffee instead of champagne! Congrats!!
that "hmm, not bad!" look at 7:57 is priceless
***** That's the look when something is disgusting but don't want to look stupid. Also, pinky up like a boss.
Out of curiosity could this process be used to extract thc from marijuana?
@Ammoniummetavanadate Sorry, it is grade 2, not grade 1. We do work with sulphides and chlorides, pure Ti is one of the only things that can reliably stand up to them.
Your video is great.
Do you know is there any commercial scale supercritical co2 extraction plant working on decaffeination for green beans in the world currelty?
Thank you
how do you know that white powder is all caffiene ? Coffee beans would also contain chlorogenic acid that could be in there also.
Good video, and work. May I suggest using redundant pressure relief safety valves (if its possible to have it to the correct pressure), a thicker viewing portal, and grinding up the coffee beans. Is aluminum a concern for leaching into the essential oil?
hey friend im shure you thought of this but have u considerd draning the co2 by using the valve on top first, to say 50 psi , imnot shure but i dont think dry ice will form at this pressure , then you coulddrain your most awsome coffee ever......
would the black staining have anything to do with a reaction with the iron in the fittings?
perhaps stainless steel might rectify this problem.
How much pressure have you taken it to before?
What camera do you use to record these? The quality is fantastic! Great project.
You crack me up. Your channel is simply the best. Thanks
did the water become acidic via carbonic acid which cause the steel create the black residue? i seem to remember playing with acids and iron and it turning black, but for the life of me cant remember much more then that.
ps, love your work
@bkraz333 that may be a bit dangerous it you end up with a extremely high percentage of pure caffeine. And how much did that shop cost to construct and what do you do for a living as i am hoping to go into the biology field?
What happens to the water when the CO2 goes supercritical?
Ridiculously impressive as always!
I find this experiment and household application of chemistry and thermodynamics to be quite interesting. I was wondering if you have an estimate on how much this scale experiment costed, where you got liquid CO2 from, and what safety precautions you had to take? I would have been quite frightened to have the pressure exceed the the working pressure of the sight glass.
Supercritical fluid extraction can be more selective than other extraction means - but I would still expect it to extract all other free base alkaloids from the coffee beans as well. This might also change the taste of the decaffeinated beans beyond just the taste component given by caffeine - AND it also means your extracted caffeine is not 100% pure - I would still be very curious what purity grade that is (and whether or not it is high - like 80-100% or much lower). Do you know anything about that?
this is awesome! can i just ask, what did u do with the pure caffeine?
can you do this for nicotine or THC?
Very awesome process and very good explanation. Congratulations on your major breakthrough. :)
Can't wait until the next vid.
You, sir, inspire me to contine on studying Bio-engineering and engineering in general
What happened to the aluminum mesh-like insert? Did it react with the supercritical CO2 as well - like in your aerogel experiment?
This has probably been mentioned but I imagine the black color was from the iron pipe you used and not the coffee beans. Have you considered using a stainless steel chamber, Though I imagine that might be a touch expensive.
I bet this guy can make some WICKED hash oil!!!
SouthernOregonOrgani you can use nearly the same way to do that and he would make shatter not oil because its more pure
it makes both. it gives you your starting material for shatter
Shut yer dam mouth you hippies! God damnit! Talking about your marijuana crack cocaine! Also, my mommy is my sister.
Note: That black pipe ships with oily protectant. It can be hard to remove completely. There's a good use for your Methyl Chloride right there !
FYI robusta coffee beans contain more caffeine than arabica beans.
Btw you're set up is awesome. I've tried the crystallized caffeine, it has a rather nasty taste.
Tannins! I remember that iron (I think a mixture of Fe(2+) and Fe(3+) is required, or maybe it's just one, I forget) reacts with tannins to produce a dark bluish-blacky ink. Iron is acidic, and takes a reasonable acid to keep it in solution, so this type of ink, though easy to make, was quite destructive to paper. I'm willing to bet your supercritical espresso shot had more than your daily dose of iron in it as well!
This is really cool. What is the efficiency of this process is w.r.t. yield?
Could the black ink possibly be the steel pipe? like making a pancake on a brand new pan, the first one always comes out black..
Why does there need to be water in the system? Is the solubility of caffeine that low in supercritical CO2? I was expecting a pipe with beans that got half filled with liquid CO2, turn it supercritical and in order to extract the solid all you would need to do would be to evaporate the CO2 leaving you with a pile of caffeine. Can supercritical CO2 not dissolve a significant enough g/ml in them compared to water?
An aqueous iron solution will turn opaque and black if tea or coffee are introduced. As it happens, that's a method of making ink, though I first learned about it by playing with 2L pop bottles of iron-rich well water adding a single drop of tea to make the whole volume slowly change.
I don't know enough about the reaction to say whether it contributed, but I figured I'd mention it for completeness.
what was the other solvent used to extract the caffeine from the black solution? you mention hydrocarbon filter,
It's awesome. As always. But I keep asking myself one question when watching your videos - what do you do for living?
Impressive work Ben
Happy new year.
Is this process is safety rather than swiss water process or sparkling water process?
I wonder how it would taste if you prepared the bean water like a normal cup of coffee? Would it also work with tea, perhaps?
Great, have you tried swiss water process decaf?
What would happen if you used roasted coffee? wonder how it would taste
Cool setup and video. Can I ask why you did all of this?
how would you test purity. it's white powder, could be sugar.
So. Did you rack up a line, or what?
what would happen if you ate that pure caffine
coming up.... from Ben - One RTG battery using just pipe fittings. I'm pretty confident you are going to end up the richest DIY guy on this planet...
No. Did you just make that up on the spot? From wikipedia: "Part of the reason caffeine is classified by the Food and Drug Administration as GRAS (generally recognized as safe) is that toxic doses (over 1 gram for an average adult) are much higher than typically used doses (less than 500 milligrams)."
Ben, I wanted to know if you knew how Avitae have made their caffeinated water that tastes just like pure water?
Awesome channel. have you made a grinder?? 😁
How do you know you have extracted caffeine and not some other compound?
You could use this process for super clean honey oil. I wonder if people have tried yet?
+tom long Yes, Its called co2 oil, legal states have ton of it to the point the rec shops stopped carrying non-co2 based oil.
+Kyle S (MrStonedOne) if that's true then that cool lol. I didn't know about the surplus of such quality.
With the pressure vessel you made from aluminium and acrylic, would the liquid CO2 leak out over large time scales? or is it reasonably stable? IE: could I make one and have a really cool workshop ornament?
Max Mouse He has a video from October 2011 answering that exact question.
Why? Emil Fisher did this extraction with water and you can modify it with alcohol and put that extract directly on the HPLC :)
You should know that Teflon tape does not seal the pipe, its purpose is to facilitate (as a dry lubricant) the screwing of the taper pipe threads, thus allowing for a better seal.
You should know that he's using steel pipe, pretty sure they have tapered threads.
It would be cool to send it in to get it tested via HPLC or something similar to see how pure it is.
Kryko I'd say the easiest quick & dirty test would be thin layer chromatography against a pure caffeine standard.
Spinning the object onto the drill bit instead of the other way? Madness.
@sabamacx Well since he based the procedure off a patent it's a pretty safe bet. I'd imagine that the patent proved that the product was caffeine (i.e. through chemical analyses such as qualitative features, TLC, mass spectrometry, or NMR spectroscopy).
Where can I find and view patents? Is it free to view them?
did you clean your extraction vessel thoroughly first and was it made totally of materials inert to your solvent?
Did you try extracting THC using this nice device? :D
This look perfect for making oil!
Reth Tard thats what i wanna kno about tbh
Hi Ben, where do you learn all this? Thank you.
@bkraz333 so does that mean you have the tf2 valve weapons?
could the liquid be black from the pipe coating?
This video is actually very informative. Thanks for putting it up.
so weird it came out black.
did you scrub out the pipe? maybe some of the black oxide coating was dissolved in the process
You have the best job in the world!
Hey, when is episode 3 coming out? :D
Great experiment. Do you think that milling the coffe beans would have given you a bigger amount of caffeine?
Try extracting hop resin (and oil) from brewing hops.
what would you need pure caffeine for? any usage?
What's your job at Valve if you don't mind me asking?
tell me that was a 300psi site glass, holding 3000.
right on w your success!!! you must not over fill the vessels w plant matter. A plug can occur between the gauge and or valves and when you open this plugged vessel, the final threads will fail sending the top off like a cannon. the pressure difference of the blast is very lethal and anyone w in that radius is in danger. be careful and try employing safety relief valves for G.P.
What about Swiss water decaffeination?
@bkraz333 i dont mean to sound rude, but where do you get the money for all this? and where do you find the time? do you have a job?
wouldn't it work with fractional distillation
Would this work for catnip? I have access to really cheap catnip, but I wonder if extracting it with CO2 would be possible.
I'm considering running it in a ball mill to make a really fine powder before the extract, and then using some DCM might work to create a pure nepetalactone extract.
any thoughts if it was black and colored becasues of residue from the metal pipe?
soooo.... ok ill ask, have you ever expertimented with more nefreious substances in that lab of yours... i mean... all these chemicals all this know how... have you ever made any illegal substances?