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Registered Member #79
Joined: Thu Feb 09 2006, 11:35AM
Location: Arkansas
Posts: 673
OK, I tried Andrew's ferrofluid tutorial and I've got some problems. I created the ferrous chloride from the ferric chloride and that part looks right. I was very careful with my measurements, I don't know if that has to do with anything. Here's what happened:
After I combined the ferrous choloride and the ferric chloride, I was supposed to add ammonia which was supposed to create magnetite which I was expecting to be black. In my first batch I never saw any black that I can remember, just looked like VERY iron rich water(rusty). Nobody on the net had pics of this stage, so I thought maybe that was normal and as I evaporated the ammonia it would change to black. So, I was supposed to cook it down until the ammonia smell went away, but after the ammonia had all dissolved in the red sludge, there was no smell any more even after heating. I have since learned that this red sludge is ferric hydroxide?
Starting over again, I was able to create black(magnetite?) by adding the ammonia to the ferrous/ferric chloride solution, but it turned red as soon as I saw a little trace of it. This is not what is supposed to happen right?
It might be important to note that I am using olive oil instead of oleic acid, but that doesn't seem to be the problem. I was able to finally work some ferrofluid out of the "ruined" batches by adding ammonia after the mixture was covered in kerosene( the carrier) and then boiling it(which was not recommended). I also now had the ammonia smell and I boiled it until it was gone. This resulted in ferrofluid that works, but no spikes and it gets clumpy, but it does slide around and follow a magnet. I think this (clumping) is because my particles are too big and I think that's because I didn't succeed with the initial precipitation. But, the olive oil in place of the oleic acid seemed to work fine.
Registered Member #79
Joined: Thu Feb 09 2006, 11:35AM
Location: Arkansas
Posts: 673
Although any input would be greatly appreciated, I think I found the answer to the "red" problem. It seems that you need to add the ammonia over a period of several minutes, stirring, and this yields and initial "red" solution that is eventually overcome by the magnetite precipitate. I'll try that Tues if I've got time. I just slowly poured it in there while stirring. I finally found a pic, their precipitate looked really nice, black and orderly. Their product looked quite a bit better than mine too due to small particles. Maybe this will give me what I want...
Registered Member #53
Joined: Thu Feb 09 2006, 04:31AM
Location: Ontario, Canada
Posts: 638
My girlfriend has been attempting ferrofluid for a few days now and has been getting better and better results. I will talk to her tomorro and find out if she has any tips on making it work.
Registered Member #79
Joined: Thu Feb 09 2006, 11:35AM
Location: Arkansas
Posts: 673
I know. It's 83% oleic acid according to my friend who is a chem teacher and a pharmacist I talked to. She said to go ahead and try it. I don't think that's the problem (at least not yet). The the crappy ferrofluid I got after I added ammonia to the "finished" batch and boiled was attached just fine to the kerosene. I made one batch without the oil to see if it was interfering with the ammonia thing, and the kerosene behaved completely differenty(It just floated on top). Duh, I know, but I was testing something and just went ahead and poured in the kerosene to see what would happen.
Registered Member #79
Joined: Thu Feb 09 2006, 11:35AM
Location: Arkansas
Posts: 673
Huh. Didn't know that. Can I get the oleic out? I'm having trouble finding it in my area. BTW I'd prefer not to do it this way: (They said it's from the middle ages or something)
"To procure oleic acid, treat oil of bitter almonds with caustic potash, and to the soap formed add hydrochloric acid; this separates the oleic and other acids. To the decomposed mixture add about half its weight of oxide of lead, and digest for 2 or 3 hours, at a temperature of 100° C. (212° F.), by which means oleates of the fatty acids are formed. Ether is now added, which dissolves only the oleate of lead; the ethereal solution is mixed with an equal volume of water, to which hydrochloric acid is added as long as is required for decomposition, and the mixture is then well shaken. The ether rises to the surface, holding the oleic acid in solution; decant it and distill it off; there remains a compound of pure oleic acid with oxidized acid. By subjecting this compound to a temperature of about -7.2° C. (19° F.), the pure crystals of oleic acid form, while the oxidized acid remains in solution. "
EDIT+> Are you getting the idea I don't know much about chemistry? Learning more about the oleic acid in olive oil... Only 1% of extra virgin olive oil is free oleic acid, oleic acid still makes up 83% of olive oil, but like robert said, it's the ester and it's tied up in there somehow. Rancid olive oil is up to 24% free oleic acid. Oleic acid can be made from olive oil supposedly easily, but I've yet to find the answer on the internet. Everybody just seems to know how to do it. This much I know: something about HCl, mix it in making sure the solution is acidic, add kerosene? Something about purifying the mixture with the crap you just poured off and something about carboxylic acids. I guess, I don't know, it's kind of put together at this moment. I know it can't be hard to make, people have been making soap with it since dirt apparently. But I can't stand to buy it it's kinda expensive for the 5mL I need. Maybe I need to talk to Granny Clampett...
Another Edit+> Over at the chem fourms, someone suggested filtering the finished ferrofluid with filter paper. According to him, he's made "spikey" ferro-fluid at home and this is the only way to make it work. He says "any magnetite that doesn't have a death grip on the oleic acid is gonna make your ferrofluid clump and cause a mess in your container" Something to that effect.
Registered Member #268
Joined: Tue Feb 28 2006, 02:44AM
Location: Ontario, Canada
Posts: 48
I am "the gf who knows what ferrofluid is" and I have managed to purchase some real oleic acid from chemistrystore.com and have far more than I can ever use. If you would like, I can sell you some. However:
I had the same problem, the magnetite didn't react. I ended up getting ferrous chloride crystals from my ever-helpful chemistry teacher. With some math, I made up a 1.5M solution and added it to the ferric in the appropriate amounts (2:1).
I did some more research and found another way to make ferrofluid, but some of the basic reactions are the same. It is a .pdf, and can be found here. (chem.wisc.edu) When I added the ammonia, it turned black, but with stirring disappeared. I ended up added about 100mL extra - VERY slowly - to completely react it all. It turned out really dark, but surprisingly brown and not black, however I ran out of time to finish it that night.
The next day the extra ammonia had separated and was sitting on top. I poured off the ammonia and cooked the remainder, but it all clumped into a blob in the middle surrounded by what looked like water with a yellowish tinge. I dont know whether this was supposed to happen or a result of from overcooking or too much/not enough oleic... Any ideas?
After pouring the "water" off, I added the kerosene, which made about 97% of the clumps break up. This solution was kind of responsive to the magnet, but settled a bit overnight. No spikes yet though!
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