Hi Pieter >Hi Keith, >I don't know for sure whether it is FFA's or something else ( BD ? ), but >the color is black and the BD is goldish, so I think it must be FFA's.
But the proportions are really all wrong. Still, it probably is FFA, but that you can't get it to separate more than that, with only so little FFA and no separation of the glycerine and catalyst, indicates that something else is wrong. Your conclusion that the by-product is almost 100% glycerine can't be right, your previous expectations (at least half) should be about right. > > How do you know it's FFAs? The glycerine layer can continue to "leak" > > small amounts of biodiesel for some time after the process. > > > > >I expected at least half of the lot being FFA's, so I have been looking >for > > >the separation at about 50% of the volume. I don't find any NaOH at the > > >bottom. > > >My conclusion is, that the bottomlayer of the BD process is almost 100% > > >glycerine. > > > > I'm afraid I'm left wondering quite what the top layer might be, > > considering what follows. > > > > >I use 3.5 grams of lye and 150 ml methanol in the process and do not > > >titrate. > > > > Not enough lye for WVO and 25ml excess methanol (12.5% stoich for > > soy) is unlikely to be enough, especially at such low temps for only > > three hours. > > > > >The mixing takes two or three hours, just to make sure that the whole > > >reaction has taken place. > > > > Hm. > > > > >Temperature is 15¡ C or a bit more. > > > > 40 more would be better. > > > > >The oil I use is WVO ( soya ), which has been used for one or two days > > > > That doesn't mean much Pieter, it could be lightly used or very > > heavily used. Used for how many hours, at what temperature? > > >The oil has been used for about 20 hours all together at 140¡ C. In which case the basic 3.5 gm/litre of lye is definitely not enough. You should try titrating it, it's not very difficult and it would tell you a lot. Lots of info on titration here: http://journeytoforever.org/biodiesel_make.html Start here: http://journeytoforever.org/biodiesel_make.html#biodwvo Then see: Basic titration http://journeytoforever.org/biodiesel_make2.html#titrate Better titration http://journeytoforever.org/biodiesel_make2.html#bettertitrate Do you test the WVO for water content, by the way? Put a litre in a saucepan and heat it on a stove; stir it and monitor the temperature; if it starts crackling and emitting little streams of bubbles from the bottom at about 50-55 deg C it should be dewatered. If not, no problem. > > >to > > >bake fish in. > > > > So it also has some fish oil in it. > > > > >After processing, I let it stand for a week or more. > > > > Before separating the biodiesel from the glycerin layer? Or do you > > remove the glycerine layer first? What proportion of the total is the > > glycerine layer? Is it usually solid or liquid? What colour? > > >I don't separate BD and glycerin layer. I just siphon ( is that the right >word ? ) The right word, and the right technique too - when you drain from the bottom the biodiesel gets drained past any residual by-product still adhering to the lower walls and bottom and can reabsorb it. It will settle to the bottom again, but siphoning from the top is best. >the BD from the top of the lot, every time I need some BD, untill I >reach the bottom. I think you may have said so before, but how long does that take? How often do you make biodiesel, and what size batches? Settling it for a long time definitely helps. >The glycerin layer is about 15% of the total volume. I think that's about right for quite clean oil using more methanol than you do. In your case it might be too little. Titration would help to confirm that. >Not >really solid and not liquid. Somewhere inbetween solid and liquid. >The color >is black. After treating it whith phosphoric acid, the color turns a little >bit lighter. The color of the top layer is black. > > >I don't wash the BD ( > > >not that I recommend this way of working, but in my case it works OK ). > > >The pH of the BD is just over 7. > > > > Have you ever tried washing your biodiesel? I'd be interested to know > > what happens. Will you try this? Put 150 ml of your biodiesel in a > > half-litre glass jar, add 150 ml of water (preferably distilled water > > if you have it, or just tap water if not), screw the lid on tight, > > and shake it up and down violently for 10 seconds or more. Tell us > > what happens next. > >Surprised about what happened : 3 layers. The top layer must be BD ( same >color as it always is ), and than a rather thick layer of white flaky stuf, >and a layer of troubled water. pH of the BD layer is still just over 7 ( >measured with litmus paper ). I don't get any sense out of litmus paper, but other people do. How is it graded? 6-7-8 etc, or half-measures too? Try measuring the pH of the water at the bottom. How long did it take to separate into the three layers? Is the top (BD) layer clear or misty? What are the proportions of each layer? Anyway, I'd say you now have a visible measure of the extent to which the whole reaction has taken place, or perhaps hasn't. That white layer should be at most very thin, hardly more than a slick. Take heart though, it could be much worse: at least it separated. In a bad case it would have turned to mayonaisse and not separated at all. Why don't you try washing some biodiesel, Pieter? A litre or so. Do you have an aquarium air pump with an air-stone, or can you borrow one? Details here: http://journeytoforever.org/biodiesel_bubblewash.html Bubble washing It might destroy the air-stone (especially the blue ones) but they're cheap to replace. Don't try using acid in the wash for now - not that it's necessarily a bad thing as some allege, but one step at a time means less confusing results. It might also start frothing and "boil over", so keep an eye on it at first, to avoid making a mess. If that happens, stop, and tell us about it. If it goes well, follow the directions, measure the pH of the wash water after each wash, do three washes or until the wash water is neutral and clear. You can use 2-litre PET bottles for this, the kind you buy bottled water in. You need two. Cut the top off just below the lid so you can get the airstone in. Pierce a small hole (2mm) in the bottom at the edge at a corner, make sure the plastic is clean and dry, and stick a square of duct tape over the hole, pressing it down tightly. Pour in 1 litre of biodiesel, carefully pour in half a litre of water, add the air-stone, and bubble away. Stand it in a saucepan or something in case it leaks or froths over. After maybe 4 hours (maybe less for the first wash), switch off the bubbler, let the water settle to the bottom. Hold the bottle over the sink, carefully pull off the duct tape and drain off the water; when it reaches the biodiesel, put your finger over the hole. Pour the biodiesel into the second bottle, prepared in the same way, continue with the second wash. Meanwhile wash the first bottle, cover the hole with new duct tape, and use it for the third wash. I'm not trying to push you into washing your biodiesel as a standard practice (though we do strongly recommend that), these are just tests to find out more about your product and the problems you're having separating the by-product. I won't try to push you into using a more standard practice either. I'd hope that you could achieve worthwhile improvements in the product by making some small adjustments rather than major changes to your way of doing it. Other people using different oils and in different circumstances might not get it to work so well, but that's not your problem, and you didn't recommend it. Beste wense Keith > > I know some people have difficulty separating the by-product layer, > > it's not only you, I've had off-list enquiries too, but I don't > > understand what the problem might be. I've tried it with different > > types of oil, with good oil and very bad oil, with at least three > > different biodiesel processes and two different catalysts, and it > > works every time, there's no difficulty at all, I can't get it to > > fail. So I can't help thinking something else must be wrong. > > > > Beste > > > > Keith > > > > > > >Met vriendelijke groeten, > > >Pieter Koole > > >Netherlands ------------------------ Yahoo! Groups Sponsor ---------------------~--> Buy Ink Cartridges or Refill Kits for your HP, Epson, Canon or Lexmark Printer at MyInks.com. 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