-I have a 160 ltre batch that will not separate, and or process
-started with wvo of questionable quality, at least 4 years old, smelly and black. This oil Ted at 14 so I did the normal acid treatment. After settling for two days, I drained about 4 ltrs of black junk and proceeded with two by-product treatments to try and clean the oil.
-first mistake, complacency, I guessed the T at 1.5 and proceeded with base processing using 1700 gr KOH in 16 ltr of methanol, nothing happened . checked the ph of the chemical/wvo mix, bang on 8.5. then the first reprocess, 2ltr methanol and an additional 240 gr of KOH, process same dismal result. Checked the ph of the mix again, 8.8 this is for sure caustic enough to geter done so what’s up?
-I did TWO more reprocesses, adding only methanol (2ltr each time) and still nothing. Did a 3/27 LOL shows ) reaction ie, 3ml dropout. What to do from here? Should note this wvo was extra dry and process temp was 140f. could it be that the by-product washes stole the methanol that was added for the AE treatment? Tom

This message has been edited. Last edited by: Biotom,

Tom,
Have you ever had to "force seperation"? I have had several batches of high titration stuff that would not seperate after reprocessing and adding more and more ingrediants. The mixture just gets thinner and thinner until the excess methanol stratifies to the top. If you take a 1 liter sample and add a few tablespoons of glycerine it may trigger seperation.
Give it a try.

-Dave-

Dave

-Yes I've done that in the past, but I don't think this batch is processed at all, even though the caustic was bang on 8.5. at least thats what I get from the 3/27, that was a joke, never seen the likes of it. Guess I will have to do some 1 ltr tests tommorrow, don't have much room left in the processor. Right now, I'm up to 25% methanol, and the ph is 8.8 Tom

Tom, sounds like my last bad batch, except it was a 3/27 pass. With that much methanol, Im sure you will have to force seperation once you do get a pass. Let us know how it goes.

-as you guys suggested I forced the separation in a test batch, using 1/3 by-product. 3/27 wasn't quite as dismal, just over 1ml dropout. but there is something else in there, when I tipped the sample out there was oily residue on the glass. I mixed methanol with 1 ml of engine oil, they don't come together very well, but leave a similare residue on the glass. This wvo may be contaminated with motor oil.
-now for the next step, I will T the separated sample and see if it's worth coninueing. Tom

Tom,
Congrats on the seperation.
I'm not familiar with the oily residue from motor oil however the batches that I had to force seperation on in the past were dismal 3/27 failures that naturally required further processing. After reading your first post again it does make sense that your glyc treatment (post acid stage) could have caused a methanol deficiency, since glycerine is sort of like pac man in the equation, (the voracious big mouth gobbling up whatever it runs into). It would be interesting to find out if your glyc after the treatment contains more methanol than before the treatment. Any chance of testing this?
-Dave-

Double D
- thats premature, but thanks. I've washed this mess 4 times with by product, but there is very little oil left, maybe 50% of what I started with. Seems this wvo was decomposed to a point that it's not worth processing, that was the reason for the oily/acetone smell I thought was engine oil.
-none the less, It was a good learning experiance, if it's black and smelly don't use it, and never never do a by-product wash after the acid treatment, if you do, say good-by to your methonol!! Tom

Did you try a reprocess after the seperation? Not that theres much time to experiment around with a full batch tying up the processor . Maybe theres an SVO guy around there that will burn the rest of it. Look at the bright side though you may have reclaimed alot your methanol with all the gly treatments, especially if you were using demethed glycerine.

I have recovered a lot of rely bad veg using a baking soda water wash on the raw oil during a couple weeks of settling (1 or 2 pound of BS dissolved in a cubie of water, stir this into a barrel of oil), I have always been able to recover at least 80% or so of the oil using this process, a barrel of oil will bubble a bit for 3-5 days and make 3-4 inches of foam on the top over a couple weeks, once the foam collapses the process is finished. The top oil layer looks and smells fine but the bottom layers of crap and water would gag a maggot. This process makes soap so it may make an emulsion that will not break, I stir 4 cups of household kitchen flour into the barrel of these batches and it has always started separation over a couple days, the flour absorbs enough water to get things started and the wet flour ends up as a thin layer of pancake batter and soap just under the cleaned oil and just above the water layer.