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I have virtually no experience with high FFA oil, so consider the following comments with that in mind.

Did you actually shake the bottles after you added the methanol/catalyst mixture to the oil?

The bottles all appear to have a clear liquid on top of a darker liquid. I have experimented several times to see what would happen if I just poured the cat'/meth' mix into the bottle holding the oil. In all cases there was no mixing, and a few moments after the addition, a layer of methanol formed on top of the oil. Your pictures remind me of that.

Soap may have formed in bottles 4, 5, and 6 because of the higher catalyst concentration. This could account for the extra material in those bottles. The reaction causing soap to form is stronger than the reaction to form biodiesel. Soap formation could occur without mixing the ingredients if there is enough catalyst.

Like I said, no experience with high FFA oil. But, this is what it looks like to me.
 
Location: Illinois | Registered: 21 February 2006Edit or Delete MessageReport This Post
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Emiper,
Where are you located? Maybe someone local to you could run some test on it and see what they get? Hate to see that much oil go to waste.
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Location: Bellevue (Omaha) Nebraska | Registered: 08 September 2005Edit or Delete MessageReport This Post
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One more point.

The last bottle has a larger diameter than the other five. Therefore, the surface area of the oil-methanol/catalyst interface is greater in this bottle than the others. The larger surface area would also favor increased soap formation in this bottle.

A bottle with twice the diameter of the others would provide four times the interface area.
 
Location: Illinois | Registered: 21 February 2006Edit or Delete MessageReport This Post
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You are under-reacting. over-reacting (with KOH) would cause an emulsion layer in the middle (milk shake kinda look). You really need to get your titration correct. It's very odd that your getting such strange results from titrating. Try titrating the oil after it's been heated to 130F and stayed at that temp for a few hours (to let water settle), you might even try letting it stay at 130F overnight so that all of the water would drop to the bottom. drain 5-10 gallons, you might be surprised at the amount of water that comes out. After that, titrate a few times until you get a repeatable number. There may alos be some non-vegetable oil substances in there. I once picked up a cubie that had some motor oil in it. that pissed me off.
 
Registered: 14 August 2006Edit or Delete MessageReport This Post
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I suspect the water in your oil is causing the inconsistent titration results, or water in either your hydroxide or methanol. It could also be that this oil titrates to an even higher value than your initial results suggest, due to contamination somewhere.

I've seen the gloppy, grainy results like in your pictures with hydrogenated oils, which seem to be even more sensitive to water contamination. One batch not long ago I totally messed up by not using a titration solution made with my latest batch of hydroxide. Make a new solution with every batch, maybe even with every titration, especially if your feedstocks are changing. This compensates for different conditions of your hydroxide due to water or air contamination, and variations from batch to batch.

Many little test batches like you've done is good, but you've got to figure out why your titrations are crazy before you proceed. Until you get consistent titration results, all bets are off as to what you'll actually make.
 
Location: Colorado | Registered: 07 June 2006Edit or Delete MessageReport This Post
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I think. We settled it for a few days, than heated the oil (i suspect mostly animal fat) to 140C until it stopped popping. It was about 50C when reacted. Today we ran the oil 50/50 with good veggie oil in a different system @ 3.6g/L. Results pending. Thanks for the help...
 
Registered: 14 August 2006Edit or Delete MessageReport This Post
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emiperformance,
Your first mistake was trying to process a batch of oil without knowing its acid content.

1st. You MUST MUST MUST get your titration straight first. Without a good titration technique that returns repeatable numbers, you're screwed..
Get that straight first.

2nd. Do a quantitive water test to find out if you need to dewater or not. This is important.

3rd. Take care of 1st or you can't make bio correctly. When you get your titration straightend out, then we have a starting point. Everthing else is just a sloppy guess.

Follow this link:
http://www.biodieselcommunity.org/titratingoil/

While your there at the link, read the entire site. Twice!!.

One thing about titrating oil, make sure its all stirred up real good so that your not titrating the oil on top without knowing what's on the bottom.. Mix it up real good..


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Registered: 09 March 2006Edit or Delete MessageReport This Post
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Ok. We worked with a more experienced fellow on our batch of the 50/50, using his tried method on our 40gal batch, which he titrated as per instructions, indicating 3.6 g/l of NaOH and 20% Methanol by volume. After two hours, more pudding.
 
Registered: 14 August 2006Edit or Delete MessageReport This Post
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