371 replies to this topic

[JohnD60]

Is it correct to mix c60+oil with mechanical mixer ? By kitchen mixer at law speed for example.

We can only make educated guesses. My educated guess is that there would be a high risk of oxidation of the OO and that said oxidation could be problematic in some way. IMO a mechanical mixer adds a potential unnecessary risk and I avoid it.

[Andey]

Is it correct to mix c60+oil with mechanical mixer ? By kitchen mixer at law speed for example.

It would work. With a magnetic stirrer, you can cover the top of the container with plastic wrap, or even put a lid on it. With a mechanical stirrer, this is harder, but not impossible. One of the pathways for adduct formation requires oxygen, so it might be a good idea to at least vent the mixture occasionally.

I ve looked at magnetic stirrers, but cheap models are very limited for viscosity of liquid, so they probably will break soon. I believe mechanical stirrers do not have this problem.
Am I understand you right that oxygenation is not a problem and I could mix it with open container ?

[zen]

Is it correct to mix c60+oil with mechanical mixer ? By kitchen mixer at law speed for example.

It would work. With a magnetic stirrer, you can cover the top of the container with plastic wrap, or even put a lid on it. With a mechanical stirrer, this is harder, but not impossible. One of the pathways for adduct formation requires oxygen, so it might be a good idea to at least vent the mixture occasionally.

I ve looked at magnetic stirrers, but cheap models are very limited for viscosity of liquid, so they probably will break soon. I believe mechanical stirrers do not have this problem.
Am I understand you right that oxygenation is not a problem and I could mix it with open container ?

After burning two Hanna's stirrers I switched to Benchmark Scientific H4000-S.
I have used it to stir 1.5 l of olive oil with no problems, I have bought mine on Amazon:

http://www.amazon.co...benchmark 4000s


I am using it together with Magnetic Stir Bar Octahedral 3" x 1/2"
http://www.amazon.co...ils_o00_s00_i00

HTH

[niner]

Is it correct to mix c60+oil with mechanical mixer ? By kitchen mixer at law speed for example.

It would work. With a magnetic stirrer, you can cover the top of the container with plastic wrap, or even put a lid on it. With a mechanical stirrer, this is harder, but not impossible. One of the pathways for adduct formation requires oxygen, so it might be a good idea to at least vent the mixture occasionally.

I ve looked at magnetic stirrers, but cheap models are very limited for viscosity of liquid, so they probably will break soon. I believe mechanical stirrers do not have this problem.
Am I understand you right that oxygenation is not a problem and I could mix it with open container ?

I think you're right about mechanical stirrers, although there are some expensive magnetic stirrers that seem to be ok. There are a couple different ways the adduct can form, and one of the important ones involves an epoxide intermediate. The oxygen in the epoxide has to come from somewhere- presumably it's atmospheric O2. I wouldn't be real happy with a large opening, just because dust and other junk might get in. On the other hand, an airtight seal might be counter-productive. It appears that all of the things we would normally want to avoid with olive oil- heat, light, and oxygen are things that encourage adduct formation. I'm not sure how you would figure out how much of any of these was the "right" amount, and how much is too much, but it seems likely there is such a thing as "too much" here. I just don't know what it is.

Has anyone run a C60 olive oil reaction that was kept cool, sealed, and dark the entire time? If so, did it develop a deep reddish color?

[Andey]

After burning two Hanna's stirrers I switched to Benchmark Scientific H4000-S.
I have used it to stir 1.5 l of olive oil with no problems, I have bought mine on Amazon:

http://www.amazon.co...benchmark 4000s


I am using it together with Magnetic Stir Bar Octahedral 3" x 1/2"
http://www.amazon.co...ils_o00_s00_i00

HTH

Thanks you for experience ) I hope after your info nobody will buy this Hanna stirrer for such work and community will save their money )
And Benchmark Scientific H4000-S is a way to go/
For me I stick to idea of trying kitchen equipment ) its easy to buy with needed features and its usable in everyday life too )

Edited by Andey, 26 September 2012 - 10:14 AM.

[hav]

Has anyone run a C60 olive oil reaction that was kept cool, sealed, and dark the entire time? If so, did it develop a deep reddish color?

I keep my 1L mix beaker sealed in a zip-lock bag in my cool dark dehumidified basement during the mix period. Keep it sealed to keep dust and insects out. Although I do flip the lights on briefly to check on it a couple times a week and make no effort to purge or displace the air in the bag. It does show the deep red color when I shine a white led-beam through it after 2 weeks of mixing.

My latest batch was pre-filtered before mixing. Should be done mixing early next week after which I'm going to filter again to see if anything is visible on the filter membrane surface.

Another thing about the autofil setup. I've been seeing cracking in their 1L plastic bottles even below 10 in of hg vacuum. Even though the docs say they should be good to 15. Noticed it during the pre-filtering when I tried doing 2L and only made it to about 600 ml before the crack happened. Changed the bottle and the 1400 ml left made it through without a crack. I've since picked up some 500 ml GL-45 kimax glass bottles which screw on perfectly. The bottles are a little too tall, however, to use the autofil quick-connect pedestal but the filter part works fine without the pedestal. Wonder if Corning, Whatman, Nalgene, or TGSI might be more crack resistant.

Howard

[Turnbuckle]

Has anyone run a C60 olive oil reaction that was kept cool, sealed, and dark the entire time? If so, did it develop a deep reddish color?

I keep my 1L mix beaker sealed in a zip-lock bag in my cool dark dehumidified basement during the mix period. Keep it sealed to keep dust and insects out. Although I do flip the lights on briefly to check on it a couple times a week and make no effort to purge or displace the air in the bag. It does show the deep red color when I shine a white led-beam through it after 2 weeks of mixing.

My latest batch was pre-filtered before mixing. Should be done mixing early next week after which I'm going to filter again to see if anything is visible on the filter membrane surface.

Another thing about the autofil setup. I've been seeing cracking in their 1L plastic bottles even below 10 in of hg vacuum. Even though the docs say they should be good to 15. Noticed it during the pre-filtering when I tried doing 2L and only made it to about 600 ml before the crack happened. Changed the bottle and the 1400 ml left made it through without a crack. I've since picked up some 500 ml GL-45 kimax glass bottles which screw on perfectly. The bottles are a little too tall, however, to use the autofil quick-connect pedestal but the filter part works fine without the pedestal. Wonder if Corning, Whatman, Nalgene, or TGSI might be more crack resistant.

Howard

You might try the 500 ml autofil instead.

[DeadMeat]

It appears that all of the things we would normally want to avoid with olive oil- heat, light, and oxygen are things that encourage adduct formation. I'm not sure how you would figure out how much of any of these was the "right" amount, and how much is too much, but it seems likely there is such a thing as "too much" here. I just don't know what it is.

At least at 150°C I assume its really toast, so probably no C60-oo pancakes.
From Cataldo's chapter 13 page 332.
www.owndoc.com/pdf/solubility-of-fullerenes-in-oil.pdf

The new absorption band at 435 nm in the C60 spectrum has been attributed to the 1,2 addition to the fullerene cage to the fatty acid chains either across to the double bonds by a Diels-Alder addition or, more simply, by radical addition (Cataldo and Braun, 2007). Thus, fatty acid esters are able to not only dissolve C60, but also react with this molecule causing the addition of the fatty chain to the fullerene cage. In fact, the bands at 435 nm shown in Fig. 13.3 appear only when C60 is stirred at 75°C for a couple of hours in the esters of fatty acids. Only for olive oil the new band appears much weaker than in the other cases and displaced at 450 nm (Fig. 13.3B). Since this oil contains chlorophyll, the displacement may be probably due also to a charge–transfer interaction between C60 and chlorophyll or with other impurities.

On standing in air, at room temperature the C60 fullerene solutions in vegetable oils are not stable, but change their colour from violet to reddish. The electronic absorption spectra show a gradual increase in the absorption band in the visible initially in the range between 450 and 550 nm. Similar results are obtained both by heating the solutions in air or under nitrogen. In the latter case prolonged heating is needed to achieve the same results. Heating C60 solutions in linseed or other oils for 15 minutes at 150°C (in air) causes the entire spectrum of C60 in the visible to disappear completely as shown in Fig. 13.3F.

[BobSeitz]

My first foray into the world of DIY C60oo production began about a month ago when I purchased a liter of Bariani's green-olive olive oil, and two grams of SES Research' 99.9%-pure C60. (If I were doing it again, I'd wait until October to try to buy Bariani's Fall, 2012, olive oil, or until late November to buy a bottle or two of the California Olive Ranch Limited Reserve olive oil, and I'd buy SES' 99.95% vacuum-oven-dried Carbon 60.)

I added ½ gram of C60 to my liter of oil, aiming for a concentration of 0.5 mg/ml.

I bought a Hannah 190M stirrer based upon an early link to this stirrer on Amazon. (It hasn't burned out so far, but I'm handling it with kid gloves.) (If I ever order another stirrer, I'll heed the latest advice and buy a Benchmark H4000-S stirrer.)

I also made the mistake of pouring my Bariani olive oil into a one-liter Erlenmeyer flask, and then throwing away the empty Bariani olive oil bottle. (What was I thinking?) The problem with the Erlenmeyer flask is that the bottom is slightly convex. That means that the undissolved C60 and the stirrer settle into the outer circle on the bottom. When the stirrer starts up, it kicks any local undissolved C60 somewhere else on the outer circle, and proceeds to rotate at the outer edge of the bottom of the flask. (This may lead to a lower back-torque on the magnetic stirrer, helping to keep the Hannah 190M from burning out. Also, I'm the stirrer at less than full speed. But the C60 is disappearing with glacial speed.) It will be three weeks tomorrow, and my olive oil has gone from whiskey-colored to deep orange, tending toward deep red in the all-but-opaque wider part of the flask.

A few hours ago, I received a one-liter, flat-bottomed Florence flask in the mail, and I'm getting ready to pour my mixture and my stirring bar into it. I'm hoping that I'll get much better stirring action that way.

Monday, frustrated with the slow progress of my green olive oil attempt, I bought a half-liter bottle of allegedly-100% Italian olive oil from a local health-food store. I poured 400 mg. of my C60 supply into the bottle, and put it on another stirrer that I also bought locally. By now, it's also turned opaque, but it's still brownish.

In an effort to find a dark environment for my olive oil that affords electric plugs for the stirrers, I've put cardboard boxes over them to keep out ambient light, and am keeping them in the computer room.

(Stay tuned for future exciting episodes of this thrilling saga.)

[zorba990]

My first foray into the world of DIY C60oo production began about a month ago when I purchased a liter of Bariani's green-olive olive oil, and two grams of SES Research' 99.9%-pure C60. (If I were doing it again, I'd wait until October to try to buy Bariani's Fall, 2012, olive oil, or until late November to buy a bottle or two of the California Olive Ranch Limited Reserve olive oil, and I'd buy SES' 99.95% vacuum-oven-dried Carbon 60.)

I added ½ gram of C60 to my liter of oil, aiming for a concentration of 0.5 mg/ml.

I bought a Hannah 190M stirrer based upon an early link to this stirrer on Amazon. (It hasn't burned out so far, but I'm handling it with kid gloves.) (If I ever order another stirrer, I'll heed the latest advice and buy a Benchmark H4000-S stirrer.)

I also made the mistake of pouring my Bariani olive oil into a one-liter Erlenmeyer flask, and then throwing away the empty Bariani olive oil bottle. (What was I thinking?) The problem with the Erlenmeyer flask is that the bottom is slightly convex. That means that the undissolved C60 and the stirrer settle into the outer circle on the bottom. When the stirrer starts up, it kicks any local undissolved C60 somewhere else on the outer circle, and proceeds to rotate at the outer edge of the bottom of the flask. (This may lead to a lower back-torque on the magnetic stirrer, helping to keep the Hannah 190M from burning out. Also, I'm the stirrer at less than full speed. But the C60 is disappearing with glacial speed.) It will be three weeks tomorrow, and my olive oil has gone from whiskey-colored to deep orange, tending toward deep red in the all-but-opaque wider part of the flask.

A few hours ago, I received a one-liter, flat-bottomed Florence flask in the mail, and I'm getting ready to pour my mixture and my stirring bar into it. I'm hoping that I'll get much better stirring action that way.

Monday, frustrated with the slow progress of my green olive oil attempt, I bought a half-liter bottle of allegedly-100% Italian olive oil from a local health-food store. I poured 400 mg. of my C60 supply into the bottle, and put it on another stirrer that I also bought locally. By now, it's also turned opaque, but it's still brownish.

In an effort to find a dark environment for my olive oil that affords electric plugs for the stirrers, I've put cardboard boxes over them to keep out ambient light, and am keeping them in the computer room.

(Stay tuned for future exciting episodes of this thrilling saga.)

I'm waiting for the new harvest green olive oil as well so excited to see someone else interested in that.
My understanding is that these stirrers work by spinning a teflon coated magnet in the bottom of the beaker. Is there any reason I couldn't drop the magnet directly in the Bariani bottle, put the top back and and stir it that way? Everyone seems to be doing the stirring with a wide open top - why is that? Does the adjunct produce a gas or something that needs to vent? If not then it just seems like inviting oxidation of the oil. Is oxidation required to produce the adjunct?

Also found this which looks cool in case you don't want to use teflon:
http://www.amazon.co...2/dp/B0048LNQJE

Edited by zorba990, 29 September 2012 - 02:45 AM.

[niner]

I'm waiting for the new harvest green olive oil as well so excited to see someone else interested in that.
My understanding is that these stirrers work by spinning a teflon coated magnet in the bottom of the beaker. Is there any reason I couldn't drop the magnet directly in the Bariani bottle, put the top back and and stir it that way? Everyone seems to be doing the stirring with a wide open top - why is that? Does the adjunct produce a gas or something that needs to vent? If not then it just seems like inviting oxidation of the oil. Is oxidation required to produce the adjunct?

Also found this which looks cool in case you don't want to use teflon:
http://www.amazon.co...2/dp/B0048LNQJE

I see no problem with putting the stir bar in the olive oil bottle, if the shape of the bottom of the bottle is right. Sometimes the bottoms of bottles are domed, so you might have a tough time with it. Adduct formation doesn't produce a gas, and doesn't need to be vented, but at least one of the pathways by which it's formed involves oxidation, so you might actually want to vent it for that reason. I would keep it at least loosely covered, just to keep junk out of it, if nothing else.

Teflon is very inert at these temperatures; are you worried about stray monomers or plasticizers?

[JohnD60]

I stirred my C60 with my Hanna magnetic stirrer directly in the California olive ranch bottle with the cap on. I did not at the time give any thought to providing additional air, but the roughly 20cc of air trapped in the top of the bottle would seem to me to be more than adequate to assist the C60/OO formation since very little C60 was used, but i could be wrong. Stirred fine, and since the bottle was square sharped, I could lay it on its side and stir it that way from time to time, thereby getting the entire contents mixed rapidly. Bob, thanks for the heads up on the heads up on COR Limited Reserve available in Nov.

Edited by JohnD60, 29 September 2012 - 05:00 PM.

[zorba990]

I'm waiting for the new harvest green olive oil as well so excited to see someone else interested in that.
My understanding is that these stirrers work by spinning a teflon coated magnet in the bottom of the beaker. Is there any reason I couldn't drop the magnet directly in the Bariani bottle, put the top back and and stir it that way? Everyone seems to be doing the stirring with a wide open top - why is that? Does the adjunct produce a gas or something that needs to vent? If not then it just seems like inviting oxidation of the oil. Is oxidation required to produce the adjunct?

Also found this which looks cool in case you don't want to use teflon:
http://www.amazon.co...2/dp/B0048LNQJE

I see no problem with putting the stir bar in the olive oil bottle, if the shape of the bottom of the bottle is right. Sometimes the bottoms of bottles are domed, so you might have a tough time with it. Adduct formation doesn't produce a gas, and doesn't need to be vented, but at least one of the pathways by which it's formed involves oxidation, so you might actually want to vent it for that reason. I would keep it at least loosely covered, just to keep junk out of it, if nothing else.

Teflon is very inert at these temperatures; are you worried about stray monomers or plasticizers?

Thanks Niner. I was more concerned that the mechanical action would break off small pieces of the teflon over time, or that the olive oil and/or C60 would draw it off with some kind of solvent action.

[Andey]

At the end of the day I choose not to use mechanical mixer and bought some entry level magnetic stirrer VELP MST.
By docs it can stir up to 5l of water...but it looks so tiny and lightweight so I am not quite sure in this numbers )
Also I bought 7cm*1cm magnetic bar and I think I made some mistake because at high speed for unknown reasons bar starts shake and at end stick to one side of flask stop rotating.
Some times it didnt happen and bar create a nice consistent whirlpool. So I leave it at low speed (pre whirlpool state) what is safe for stoping reasons )
I received 2g of SES 99.5% C60, take approx halа of a gram and started a batch with 0.75l olive oil.

[Andey]

Solution was getting really dark with some red and brown tint. Still a lot particles flowing but much less than on beginning.
I can not see stir bar but it working )

Is it looks ok for about 15 hours stirring ?

[niner]

Wow, that reacted very quickly. Most people stir for 10-14 days or so. The problem with your stir bar is the length to width ratio is too large. You would be better off with a shorter bar, or a hexagonal or octagonal bar. Considering how things are working for you, the bar might not matter. I'd just keep stirring it, and wait to see if your C60 particles disappear. If it's a low purity C60, which it might be, considering how quickly it's dissolving, then you might get some persistent particles of non-fullerene soot that never go away.

[Andey]

Wow, that reacted very quickly. Most people stir for 10-14 days or so. The problem with your stir bar is the length to width ratio is too large. You would be better off with a shorter bar, or a hexagonal or octagonal bar. Considering how things are working for you, the bar might not matter. I'd just keep stirring it, and wait to see if your C60 particles disappear. If it's a low purity C60, which it might be, considering how quickly it's dissolving, then you might get some persistent particles of non-fullerene soot that never go away.

For me it looks like reaction speeds up when i shake it, so many air bubbles occur in solution.
May be its not a common situation - because of low speed stirring a lot of particles lands on bottom so I had to shake it vigorously (first time 3 hours after start stirring, and 2 times after) and after this solution quickly starts to darken.
I think you are right about bar size. In stirrer manual I found recommended bar size 6*35mm or 6*20mm - its way less than I bought. So after this batch I will buy right one bar. Here in Ukraine we have an expression for such thing - there is no rest for legs with stupid head ))

Edited by Andey, 09 October 2012 - 01:18 PM.

[Turnbuckle]

Most people stir for 10-14 days or so.

I stir (magnetically) for 3 days with C60, 1 day or less for C60/C70.

[niner]

Most people stir for 10-14 days or so.

I stir (magnetically) for 3 days with C60, 1 day or less for C60/C70.

That's really quick. The C60/C70 makes sense, because it should dissolve a lot more quickly due to lower lattice energy. (A mixture of spheres (C60) and ellipsoids (C70) can't pack as tightly as pure spheres.) What's the purity of your C60? I'm using the vacuum-baked 99.95% from SES, and it is taking forever! In fact, I just bought a nice mortar and pestle so that I can grind the C60, then I will try a new batch. The mortar came from my favorite laboratory equipment supplier, Bed Bath and Beyond. Twenty bucks. Aside from my suspicion that the 99.95 takes longer to dissolve, I also inadvertently used olive oil from a large container that I had added a bunch of vitamin E to. I suspect that's slowing things down as well. This time, I'm using a clean bottle of oil. As before, this batch will be in the James Bond style- Shaken, not stirred. We'll see how it goes.

[Turnbuckle]

Most people stir for 10-14 days or so.

I stir (magnetically) for 3 days with C60, 1 day or less for C60/C70.

That's really quick. The C60/C70 makes sense, because it should dissolve a lot more quickly due to lower lattice energy. (A mixture of spheres (C60) and ellipsoids (C70) can't pack as tightly as pure spheres.) What's the purity of your C60? I'm using the vacuum-baked 99.95% from SES, and it is taking forever! In fact, I just bought a nice mortar and pestle so that I can grind the C60, then I will try a new batch. The mortar came from my favorite laboratory equipment supplier, Bed Bath and Beyond. Twenty bucks. Aside from my suspicion that the 99.95 takes longer to dissolve, I also inadvertently used olive oil from a large container that I had added a bunch of vitamin E to. I suspect that's slowing things down as well. This time, I'm using a clean bottle of oil. As before, this batch will be in the James Bond style- Shaken, not stirred. We'll see how it goes.

I use 99.5% C60, and yes, that will likely speed things up.

[niner]

I just bought a nice mortar and pestle so that I can grind the C60, then I will try a new batch. The mortar came from my favorite laboratory equipment supplier, Bed Bath and Beyond. Twenty bucks. Aside from my suspicion that the 99.95 takes longer to dissolve, I also inadvertently used olive oil from a large container that I had added a bunch of vitamin E to. I suspect that's slowing things down as well. This time, I'm using a clean bottle of oil. As before, this batch will be in the James Bond style- Shaken, not stirred. We'll see how it goes.

Wow, it is working spectacularly well, if the color of the mixture is any measure. The C60 I'm using (SES 99.95%) is fairly granular. I cleaned and dried the mortar and pestle, and proceeded to grind the C60. It was fairly soft and easy to grind, and quickly formed a shiny black smear on the porcelain surface of the mortar. I scraped it onto a sheet of paper, which was probably a bad choice for something so finely divided. Next time I might try a sheet of glass. A lot of it seemed to stick to the mortar, although that might have been a case of a little bit of something the color of C60 looking like a lot. I put some olive oil in the mortar and ground it to mobilize the remaining C60, then spooned it into the bottle. This was a messy procedure that could be improved upon. Once most of the C60 was in the storage bottle, it was obvious that the grinding had made a huge difference, compared to the bottle that had not been ground. The ground C60 hung in the solution, and even several hours later had not fully settled. The kicker is that the red/purple color is already developing rapidly. This could be a low cost alternative to a magnetic stirrer.

Here's the model I used.

[niner]

I just wanted to post a shot of the results at 24 hours of using ground C60 instead of crystalline. The color is developing very nicely. This is a shot holding a clear glass 750ml bottle up to the sky. The camera is fairly close in order to get the bottle to fill the frame and not be washed out by the sky, so as a result, it's a little out of focus even though I used a macro setting. I just wanted to show the color though. This was not stirred, only shaken several times. It was stored at room temp in a dimly lit room. Grinding the C60 seems to speed up the process by an order of magnitude or more, which makes sense if dissolution is the rate determining step.


 c60-oo-24hrs.jpg   137.45KB   17 downloads

[Turnbuckle]

...I put some olive oil in the mortar and ground it to mobilize the remaining C60, then spooned it into the bottle. This was a messy procedure that could be improved upon...

Here's the model I used.

Perhaps if you went stainless...

[zorba990]

I just wanted to post a shot of the results at 24 hours of using ground C60 instead of crystalline. The color is developing very nicely. This is a shot holding a clear glass 750ml bottle up to the sky. The camera is fairly close in order to get the bottle to fill the frame and not be washed out by the sky, so as a result, it's a little out of focus even though I used a macro setting. I just wanted to show the color though. This was not stirred, only shaken several times. It was stored at room temp in a dimly lit room. Grinding the C60 seems to speed up the process by an order of magnitude or more, which makes sense if dissolution is the rate determining step.


 c60-oo-24hrs.jpg   137.45KB   17 downloads

Very cool! I see this is referenced here : http://www.xbr.jp/yo...ne/index_e.html
as a method of water dispersion.

I suppose the chance of actually breaking the C60 cages with the process is nil?

[niner]

Perhaps if you went stainless...

Yeah, I saw that one on the web site, but they didn't have it in the brick and mortar store where I got the porcelain set. I wonder how it would perform? Probably pretty good since it has a brushed surface, so it wouldn't be too smooth, but wouldn't be porous like the porcelain surface is, so it should be easier to clean.

Very cool! I see this is referenced here : http://www.xbr.jp/yo...ne/index_e.html
as a method of water dispersion.

I suppose the chance of actually breaking the C60 cages with the process is nil?

Wow, in that paper, they talk about getting 20 nm particles just from grinding. The C60 seemed pretty soft to me, and it was really easy to crush the particles to a super-fine material. So fine, in fact, that when I looked at it about four hours ago, I could only see a small wisp of particles, then a couple hours after that, I saw none. In a little over 24 hours, I think it's done! (At least as far as particles visible to the naked eye, which is pretty large, actually.) I'll let it sit for quite a while before using it, since I have to finish my store-bought c60-oo, and I'm experimenting with figuring out the minimum dose, which takes a long time. Needless to say, my other batch that's been sitting around for three weeks with no apparent reaction whatsoever is due for some work. I'm going to pour off as much of the oil as possible, grind the remaining particle/oil mixture, then replace the oil with new stuff.

[trance]

Very cool! I see this is referenced here : http://www.xbr.jp/yo...ne/index_e.html
as a method of water dispersion.

I suppose the chance of actually breaking the C60 cages with the process is nil?

Wow, in that paper, they talk about getting 20 nm particles just from grinding. The C60 seemed pretty soft to me, and it was really easy to crush the particles to a super-fine material. So fine, in fact, that when I looked at it about four hours ago, I could only see a small wisp of particles, then a couple hours after that, I saw none. In a little over 24 hours, I think it's done! (At least as far as particles visible to the naked eye, which is pretty large, actually.) I'll let it sit for quite a while before using it, since I have to finish my store-bought c60-oo, and I'm experimenting with figuring out the minimum dose, which takes a long time. Needless to say, my other batch that's been sitting around for three weeks with no apparent reaction whatsoever is due for some work. I'm going to pour off as much of the oil as possible, grind the remaining particle/oil mixture, then replace the oil with new stuff.

Are there any studies on the shearing force resistance of C60? Do all of the buckyballs stay completely intact structurally, a portion of them, or none of them, under the pressures and temperatures from the frictional force of grinding them down mechanically? Thinking beyond that, what visible color results are achieved if we dissolved carbon soot or powdered graphite in olive oil?

[niner]

Are there any studies on the shearing force resistance of C60? Do all of the buckyballs stay completely intact structurally, a portion of them, or none of them, under the pressures and temperatures from the frictional force of grinding them down mechanically? Thinking beyond that, what visible color results are achieved if we dissolved carbon soot or powdered graphite in olive oil?

Any measurement of shearing force that could be made on the macroscopic scale would involve only the disruption of the crystal lattice, which doesn't take much force at all, since a C60 crystal is like a cubic array of marbles, only held together by Van der Waals forces, and not very big ones at that. (Carbon is not very polarizable, though the aromaticity of C60 does help.) On the other hand, the forces needed to break the bonds in C60 are orders of magnitude higher, so grinding isn't going to hurt the C60. This sort of thing has been extensively analyzed for drug molecules that are a lot more fragile than C60, and also have much harder crystals.

I don't think that carbon soot or powdered graphite would dissolve in olive oil. Even C60 has a very low solubility in olive oil, but because it reacts with the fatty tails of the olive oil triglyceride, it forms a compound that is much more soluble. (About a hundred times more, IIRC.) Carbon soot and graphite would be mostly unreactive, although soot naturally contains a very small amount of C60.

[maxwatt]

I would think brushed stainless steel would have similar problems to the ceramic, as the tiny grooves brushed into the steel would trap some of the material.

An artist's muller* and a sheet of glass would probably be the ideal grinding implement, adding just enough oil to get a paste one could then pick up with with a pair of palette or plaster knives.

* a mulleris a specialized pestle designed to work with a flat sheet of glass rather than a bowl

Available here: http://www.jerrysartarama.com for less and probably elsewhere with a search engine.

I happen to have a large one in my country house but it may be too large for mixing a small quantity. You don't need the pricey frosted glass sheet, ordinary window pane glass works as well and is easier to clean up; you might want to roughen the surface by grinding some carborundum, available in some hardware stores. The entire process is illustrated here

I don't know the ratio of C60 to oil that would be ideal for making a thick paste that could be then added to the remaining oil for mixing up a batch, and I do not think we want so thick a mixture as is used to make oil paints.

Edited by maxwatt, 11 October 2012 - 02:41 PM.

[FunkOdyssey]

I wonder if you aren't reaching a level of expense and complexity with the muller'ing, strategies to reduce lost material, trying to make pastes, etc that the original magnetic stirrer approach becomes more attractive.

[trance]

I wonder if you aren't reaching a level of expense and complexity with the muller'ing, strategies to reduce lost material, trying to make pastes, etc that the original magnetic stirrer approach becomes more attractive.

I'm just letting mine passively "age" in two 500 ml bottles of Koroneïki olive oil, rotating and shaking every once in a while. Shaken, not stirred.