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messed up batch, need advice
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Ok, here's what happened. I started a batch in my processor. 375 gallons oil 5.0 ml naoh T, 35 gallons methanol, 1022 ml sulfuric(based on Dkenny's .18).
I pulled in the oil, but didn't shut the valve after doing so. I then pulled in my load of methanol, and dumped in my acid. I started processing. By the time I noticed the valve, 35 gallons of the mix had run out of the processor into my oil holding tank. I let it sit until the next morning, and retitirated. It had done something, because it titrated at 2.1.

I then added a fresh 35 gallons of methanol, and 400 ml of sulfuric. I reprocessed, mixing for 6hrs at 165F then let sit for another 6hrs. This time my numbers went up! Last night it T was at 2.5 naoh. i'm a little puzzled why it went up. do I have too much acid in this batch? Is that what is throwing off my numbers? I usually get between 1.1 and 1.4 ending T. I'm going to check it again this evening, but was hoping for some suggestions. 2.5 isn't bad, I just don't want to make a lot of soap. AE has kind of spoiled me for soap numbers at the end.


Thanks again

Rich


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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for sure the acid amount/ltr of wvo you use affects the final titration. a ball park min T would be 2 for each ml of acid used/ ltr of oil. Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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since this batch is essentially a 'do over' I have a total of 1,400 ml in 375, or about 1 ml per liter. all of my other batches have come out very good. but this one came out at higher than normal I guessed due to losing so much methanol and sulfuric due to my error. Tom, is that a drop in 2 ml of titration, or it should finish at 2? it started at 5. I have to wait until tomorrow to do an updated titration. I'll repost when I do that. thanks


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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quote:
Originally posted by Road Runner:
is that a drop in 2 ml of titration, or it should finish at 2?
It takes about 1.4g NaOH to neutralize 1ml of H2SO4 assuming a purity of 100% for both chemicals.
The titration detects the H2SO4. So, if you used 1ml H2SO4 per litre of oil, the minimum titration you could hope to achieve is 1.4, the H2SO4 used in the reaction. If you used 2ml H2SO4 per litre of oil the minimum titration would be 1.4X 2= 2.8.
 
Location: Upton | Registered: December 20, 2010Reply With QuoteReport This Post
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it should finish at 2?

yes,(2KOH) but, if you drain the sludge from the bottom after ae, T will be lower. I've had batches as low as .75T. after AE starting T9. as stated in the previous post, the effect the acid will have on finnal T will depend on the purity of the acid. Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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so far all of my ae batches haven't had any water or sludge in the bottom when I check. Our worst oil so far has been 6.8 naoh. I've been having pretty good results, but I'm getting some naoh residue throwing off my results a little. My system is all sealed, and every thing is moved from tank to tank by air and vacuum, so the only way I can bring in methanol, is by filling my methoxide mixing tank, then into the processor. the mixer is where I'm pretty sure I'm getting lye contamination. I'm working on building a new processor and methanol tank just for ae, but in the mean time I have to keep making fuel, so I just add an extra 20 ml or so to counter act the residual lye.


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post



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I got the batch in question to work out ok, it passed 3/27 with flying colors. The next batch will be a true test for me, It titrated at 10.2 ml naoh! that is the worst we have ever had. will see in the morning what I get.


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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ok, the 10.2 batch dropped to 4.8,I did base step on it. It passed 3/27, but i can see soap bits floating in the bio layer before demething. I fear this is going to make a batch of jello if I demeth it. I know why (likely water due to a processing mistake), I'm just not sure what to do as yet. should I try whole batch demeth, and hope the numbers go down, by sending some of the soaps into the glycerin layer, or do I just drain the glycerin as normal. Do I demeth the bio alone, and see what happens, or do I put the whole load back into raw oil, and take the loss? not sure what to do, we are talking about 375 gallons of fuel, so it's not like I want to dump it and start over. hmmm. every time I think this is getting routine, I step on the rake with the teeth pointing up.


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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Soap washes out, so does methanol. You might try washing a small sample with distilled water & see the results. I've not done AE yet.
 
Location: Texas | Registered: April 27, 2011Reply With QuoteReport This Post
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as dumb as this sounds, I have had zero luck with water washing. We did a little of it when we first started making fuel 3 years ago, but then I stumbled onto the whole gl process, and filtering though wood shavings, and haven't looked back. I did revisit water washing last fall, when we first got into bad oil, but the batches I had trouble with, wouldn't wash, or filter. They had an incredible amount of soap in them. those batches got drummed up for long term settling. I have a feeling if the wbd will make some of the soaps fall out with the glycerin, even some improvement will be a great help.

here's the funny thing about this batch, I did a titration on the fuel after my acid/base, and it said that it was short on lye. It did pass 3/27, but I can see bits of soap floating around all of my other batches of acid base came out exactly neutral. pink as soon as you put in the fuel, not pink with just a few drops of sulfuric titrating soulution. this batch I had to add almost 1.5 ml of naoh titrating soulution. I'm guessing it came up short because it make the soap. I don't know how this is going to work out, but I am pretty sure the processor is going to get a cleaning after this batch so it can't mess up the next batch.


powering
2 bobcats, an excavator, and a ventrac mower. looking for a diesel weedeater!
 
Location: morgantown wv | Registered: June 18, 2008Reply With QuoteReport This Post
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