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Old 02-14-2010, 07:39 PM #11
Elemental
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Smile Co2' extraction

This is a good lecture about it^^^^ in my book:

http://fullmeltbubble.com/forum/showthread.php?t=6767
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Old 02-14-2010, 07:48 PM #12
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Coupled with a fluid modifier such as toluene, dry ice-originated supercritical CO2 (Sc CO2) achieves quantitative extraction of many volatile organic compounds
No thanks. :(
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Old 02-15-2010, 04:40 AM #13
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http://www.edenlabs.org/supercritical_extraction.html
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Old 02-15-2010, 03:22 PM #14
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As my memory serves me, CO2 becomes super critical in the neighborhood of 1100 psi and 89F. Actually pretty low and easily achievable.

At the cryogenic temperatures reached as the pressure is released, carbon steel becomes a grenade, so typically 300 series stainless is used.

A piece of 4" Schedule 160 stainless pipe is more than adequate for a 1500 psi operating pressure, and still maintain a 3X safety factor.

Liquid C02 at atmospheric pressure is called dry ice, so some pressure is required to just keep it liquid.

A 50 gallon Dewar of liquid C02 with a dip tube, would allow you to pre-pressurize your vessel to ~150psi with the 250psi gaseous head pressure to keep it liquid, and still have transfer pressure using the liquid dip tube.

Per Boyles ideal gas law:

The state of an amount of gas is determined by its pressure, volume, and temperature. The modern form of the equation is:
where p is the absolute pressure of the gas; V is the volume of the gas; n is the amount of substance of the gas, usually measured in moles; R is the gas constant (which is 8.314472 J·K−1·mol−1 in SI units[4]); and T is the absolute temperature.


You can heat the reaction vessel with simple pipe heaters, to hit whatever operating pressure you wish. If a back pressure regulator is placed in the system that limits backpressure to 1500psi before venting to atmosphere, you can operate in super critical range without overpressuring and exploding the vessel.

By starting with liquid C02, it eliminates the need for pumps and a refrigeration system.

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Old 02-24-2010, 03:12 AM #15
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I am about 3/4th of the way through that patent. I'm not sure if you all have taken the time to actually read it, but it is amazing. It is a step by step guide on how to do this process at its utmost efficiency. Here is a link to the full document available for download:
http://www.google.com/patents?vid=USPAT7344736

It says that they found the optimal pressure for the CO2 extraction was actually sub-critical, not super-critical, and it goes into detail why. It's basically the same as making quality dry sift, where softer/longer = better quality and harder/faster = lower quality. Quality being determined by percentage of cannabinoids to residual plant matter in this case, though, whereas for dry sift it would be trichome heads to plant matter.

That is the most detailed and thorough document I have ever read in my life, and it just so happens to be about something I am very interested in. As I was reading I was thinking in my head that I'm sure this could be pulled off DIY style....if you were very careful and had some cash to spend. I am already picturing a little laboratory, would probably be a lot of fun. Very interesting thread.
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Old 02-25-2010, 05:47 AM #16
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Nice find hades. This info plus eden labs notes about sub-critial being better for botanical extractions should seal the deal. I guess we don't have to extract with a pipe bomb (well not a very strong one anyways). I think I want to have the option anyways. I will let you guys know what I put together.

Thanks for all the input.

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Old 02-25-2010, 05:37 PM #17
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I'm sorry I didn't get through that whole article before I posted. It turns out that they did an experiment, which is at the very end of the document, which actually does find that super-critical levels with 2% ethanol added to the liquid CO2 is actually the most efficient method. They used a high CBD strain for this experiment, but the same applies if it were a high THC strain:
Quote:
The results illustrate that changing the extraction conditions from sub-critical to super-critical increases the solvating power of the CO2 and results in a higher recovery of the available CBD. However, the supercritical CO2 can now solubilise a wider range of compounds and the extraction of these additional compound has the effect of diluting the concentration of CBD in the extract to such an extent that it is now lower than that obtained for the sub-critical extraction. Consequently, the marginal additional recovery of available CBD from the raw material would not outweigh this disadvantage and demonstrates the use of supercritical conditions is not desirable.
This coincides with the method they present in the paper, but it goes on to dispute their own claim....
Quote:
The addition of 2% w/w absolute ethanol to supercritical CO2 as a modifier increases the recovery of the available CBD to >90%. Presumably the relatively polar cannabinoid is more soluble in the extract of increased polarity.

Interestingly, the concentration of CBD in the extract is increased slightly by the addition of polar modifier. This would seem to indicate that the co-extractable non-cannabinoid material present in the plant material is less polar than the target cannabinoid and hence the extraction of this material (the "ballast") is deselected when polarity is increased.

Thus, extraction of cannabis plant material with supercritical CO2 2% w/w ethanol provides an increase in recovery of the target active with no attendant penalty of loss of selectivity.

In Summary:

1. A switch from sub-critical to super-critical conditions produces little advantage in terms of overall recovery of cannabinoid from the raw material but does result in the disadvantage of reducing the active content of the extract.

2. The addition of 2% absolute ethanol modifier to supercritical CO2 results in a significant improvement in the recovery of cannabinoid from the raw material with no penalty of dilution of active content by co-extracted material.

Last edited by hades; 02-25-2010 at 05:39 PM.. Reason: clarification
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Old 04-21-2010, 07:00 AM #18
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very interesting any updates??? im very interested
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Old 04-22-2010, 11:50 PM #19
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Originally Posted by 3dDream View Post
BTW if people have access to papers:

I don't wanna buy it.
I was thinking about designing and building some sort extractor.

I uploaded the paper plus most of its references, which includes a book, as well as two other papers that are related to C02 extraction. I can't vouch for the usefullness of these since I don't have the time to read them yet.

A high volume approach would be to buy a CO2 tank that connects to a bunch of fittings, a pressure regulator, a heating section, and a collector.

These are the critical properties of CO2

304.21 K
31.06 C
87.91 F

7.383 MPa
72.86 atm
1070.81 psi

To reach the critical point of CO2, class 600 fittings are required as per ASME B16.5. Don't know how much those cost but they aren't cheap. I'd guess you could build the project for $100-$300, but I'm not sure.

I like the idea of just using dry ice in a 15 ml centrifuge tube. It wouldn't be critical C02, but I guess that isn't a problem if you aren't supplementing with ethanol.

I need to study for exams tho. The links below are mirrors of each other. If you find another article you need just post the DOI—this one for example is doi:10.1016/j.talanta.2004.05.049—or the next best thing is the author, title, year.
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Old 04-23-2010, 09:01 PM #20
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i only dabbled into the articles so far but as i get further i will make a decision as to whether i will pursue an at home DIY version

at the moment i have a whole bunch of left over paintball co2 tanks and all kinds of fittings and steel braided line most of which is rated in excess of 3000psi

i just wanna plan out a setup before i try anything and blow something up.

im thinkin that the 12-20oz co2 tanks are going to be the best as they are cheap to fill so recovery of the intitial solvent isnt necessary. im just wondering if it would contain enough actual liquid co2 as i haveno clue as to the volume necessary.

lets keep this thread goin guys i wanna get away from the ethanol based solvents and see what i can do with this.

ill be back when im more educated on the processes already discussed
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