Saturday, September 3, 2011

A close look at supercritical carbon dioxide CO2



I built a pressure vessel from aluminum and acrylic and filled it by placing pieces of dry ice inside. The dry ice melts under high pressure, and forms a liquid and gas phase. When the vessel is heated, the CO2 becomes supercritical -- meaning the liquid and gas phases merge together into a new phase that has properties of a gas, but the density of a liquid.

Supercritical CO2 is a good solvent, and is used for decaffeinating coffee, dry cleaning clothes, and other situations where avoiding a hydrocarbon solvent is desirable for environmental or health reasons.

If you have a suggestion for what I should do with the supercritical CO2, please leave a comment.

Here are a few engineering calculations that I used to determine the pressure capacity of the chamber:

1. Hoop stress in the aluminum ring:
http://www.engineeringtoolbox.com/stress-thick-walled-tube-d_949.html
The aluminum alloy and heat treatment is unknown unfortunately, which makes a huge difference in its material properties. Since it is a structural tube, I will assume 6061-T4, which has a yield strength of about 40 ksi.

ID = 1.1", OD= 1.5" (to the inner edge of the bolt circle)
Chamber pressure = 3000 psi
Hoop stress at inner edge = 10ksi

So, there is a safety factor of 4, but the additional material outside the bolt circle will actually add to this factor. In theory, the aluminum will yield at 12000 psi chamber pressure.

2. Bending force on the acrylic windows:
Acrylic ultimate strength: 10 ksi. It doesn't yield. It is elastic, then breaks. Modulus: 400 ksi
http://www.efunda.com/formulae/solid_mechanics/plates/calculators/cpS_PUniform.cfm#Results
The plate is not a thin plate, but the results show only a 0.004" deflection at the center under a chamber pressure of 3000 psi.

http://www.xcalcs.com/cgi-bin/tutti/x3calcs.cgi?d=i_4_0_1_0_0&l=en

This shows a stress of about 4.3 ksi for a 1.25" thick acrylic plate with 1.35" radius. The pressure-bearing radius is larger than the inner radius of the aluminum ring. This has a safety factor of 10/4.3 = 2.3. In theory the acrylic will break apart when the chamber reaches 7000 psi.


3. Stress on the bolts:

Total window area is about (pi)(1.35)^2 = 5.7", so total force when chamber pressure is 3000 psi is (5.7)(3000) = 17,200 pounds! I will use six bolts, so each bolt must hold 17,200/6 = 2860 pounds.
http://www.derose.net/steve/resources/engtables/bolts.html

1/4-20 bolts are NOT strong enough -- even at grade 8!

5/16 bolts would be OK in grade 8, but I wanted a higher safety margin, and I don't like 5/16 bolts.

I chose 3/8" grade 8 bolts, which have a working load of almost 7000 pounds. I wanted to be sure bolt failure could not possibly be the failure mode that breaks the whole system. I also used grade 8 nuts, which should ensure the failure happens within the fastener, not by shearing the threads out of the nut or bolt. I am not positive about this, though.

4. Pipe threads:

I wasn't sure what 1/8" pipe threads are capable of holding, but McMaster sells such fittings that are rated for 5000 psi (like the gauge that I used), so I assume a brass part can hold such a load. I cut threads into the aluminum so it's possible that the pipe thread in aluminum could fail (ie the gauge or valve could be pushed out, shearing the threads right out of the aluminum ring). It might be possible to add up all of the area of the pipe thread cross-sectional area, but it seems silly and unlikely to be at all accurate.

5. Temperature concerns:

The acrylic has a glass transition temperature of at least 180*F, but it should not be heated anywhere near this temperature or else its ultimate strength rating may not be valid. I would say 130*F is the upper safe limit.

6. Effect of supercritical CO2 on the acrylic and O-ring:

I used buna-n O-rings, which may affected by exposure to SC CO2. They are very unlikely to fail in the short term, and I can change the O-rings for every experiment if I want.

The acrylic showed signs of crazing after just one supercritical CO2 cycle. I think the crazing is unlikely to affect the acrylic's ability to hold pressure, but there is a slight concern.


The most likely failure mode would occur when the acrylic reaches its ultimate strength, and suddenly breaks. Unlike pressure vessels made from ductile materials, which can be designed to yield and leak before breaking, the acrylic will suddenly blast apart without leaking first. If the equations and material specs are correct, 3000 psi should be OK, but I would not want to go much higher.

22 comments:

Joey Hagedorn said...

Hey Ben, Thanks for this interesting video! How do you end up safely venting the chamber, since it has no valve?

Ben Krasnow said...

Joey, it was indeed a problem: http://www.youtube.com/watch?v=M4CTkicgKtE

I added a valve, and it works well now.

Hash said...

Very cool Ben... Are the o-rings made of any special type of rubber, or just standard o-rings?

Ben Krasnow said...

Hash, I used plain buna-n O-rings. Someone mentioned the supercritical CO2 might penetrate the buna-n, and cause a failure upon decompression. I am not sure if this happened during my O-ring mishap. After adding the valve, I don't anticipate a similar problem, but it's true the O-rings may not last long in this environment.

牛晓旭 said...

Hi Ben,

A CF flange view port design with copper gasket seal should solve the O-ring problem.

Niu

RonB01 said...

Have you thought of using a bar clamp to temporarily hold pressure while you are tightening the bolts? There are some quick-clamp units with rubber facing that might work.

Nick said...

This is a really cool project, Ben. I love being able to see the stuff that's usually hidden inside metal pressure tanks.

Supercritical ethanol can be used to "see" high energy particles such as cosmic rays as with cloud chambers, I wonder if you could use co2 in the same way. You'd have to get just the right temperature and pressure where the co2 sits just above the condensation point - at least that's how the cloud chambers work.

DocN said...

Very cool setup. Makes me want to go build one. :)

One thing to watch out for, though; you mentioned trying to fill the chamber more, so you need to be very careful not to overfill it. If the liquid phase doesn't have the room to expand into the gas/supercritical stage, pressures can skyrocket rapidly.

You might consider machining the aluminum ring for a burst disc, such as from a paintball tank, for safety.

Doc.

David Eaton said...

I think I might cool the chamber in something like a dry ice/isopropanol bath. Then you could close it up before the pressure builds. Also, you can weigh the CO2... 'just toss some in' is a common approach in chemistry, but ill-advised.

If you have any worries about the bolt holes letting loose unexpectedly, why not do experiments with the chamber in a pressure cooker or other metal containment vessel? Your posts are very cool. Having you taken out by this will not do.

You can do lipid extractions from plants or from food. Extract the oil from chips or cake. See how much of the food is fat. Be horrified. Remember how good they are, and ignore your results.

David Eaton said...

I second the thoughts about burst disks, too.

Seb Zeppelin said...

Hi there,

Beautiful demo, and a nice bit of machining too!

What are the engineering formulas you used to calculate the thickness of the acrylic? also, will you share an engineering drawing or dimensions of the vessel? I'd like to have a go at making one of these, except perhaps with a valve and safety burst disc thrown into the mix.

Recently graduated mechanical engineer here, so feel free to go technical on me...

Thanks,

Sebastian.

Ben Krasnow said...

Seb, I added some engineering info to the blog post. I don't have any drawings, and the dimensions were chosen solely to suit the material that I had on hand.

I am going to try caffeine extraction, but I will be using an all-aluminum chamber with a safety disc. I will be heating it to temperatures much higher than the acrylic could handle. Stay tuned.

Let me know if you have any input regarding my engineering analysis.

Anonymous said...

Keep up the good work, Ben!

Have you thought about seals using Indium metal? Could support long-term display of liquid CO2!

How about liquid Oxygen? It would be supercritial at about 750psi, I think.

Liquid Xenon would also be doable at just below room temperature (or a fridge) at less pressure than your CO2.

Anonymous said...

Same Anon as before, I had a recommendation- Aerogels! It would be wonderful to make these with a window, most ESPECIALLY lanthanide oxide aerogels!

http://www.aerogel.org/?p=1467

Migs said...

Look up Dr. Goodling from the Mechanical Engineering department (now retired) in Auburn University. Back in 1984 he had this set up to show the triple point exactly. He could have a storm inside the vessel. Maybe he can give you some pointers and a proper clear wall material.
Regards,
Miguel Reznicek
mreznicek@pretensa.com

Anonymous said...

I think you should stop messing with your device and CO2.
Acrylic has a high affinity for sc CO2. The crazing you saw is the effect of CO2 dissolving through the acrylic window surface, and followed by the creation of bubbles when you depressurized the vessel.Under long exposure (several hours), acrylic will soften into a rubber, and the whole thing will blow up. Believe me, you don't want to be around when this happens.

Ben Krasnow said...

Anonymous, you should see my video regarding the acrylic chamber after a one-week exposure to liquid CO2, and my video that shows the aftermath of an O-ring blowout. I am building some new acrylic windows and will continue playing with things that interest me. Thanks for your concern.

Cuongktv said...

It's great! Thanks for share.
By the way, could you introduce some other transparent materials which can sustain with pressure from 3000 to 5000psi?
Thank you so much!

Anonymous said...

Your calculations are helpful in guiding design of the vessel...except for the bit where your O-ring is probably the weakest point - even if it wasn't already extruding into the space around it.

+1 for a bursting disc too.

André said...

Fantastic job!!
Off course the acrylic isn't the best(and safe) material for sc-co2 using, but it's cheap!!! and it is really cool to see someone building a high pressure view cell with these material!!!
Super!!
I'm work with SC-CO2 phase equilibria and extraction of biocompounds!

Cheers man!!!

André Zibetti

Anonymous said...

Have you thought about using thin glass panes reinforced by acrylic? Glass should be chemically inert and you won't need it for structural purposes.

co2xtractr said...

hey im at a point where o-ring failure cant happen. my vessel rating is 6,000 psi and wondered your experience w seals and what works

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