[Biofuel] Bad Week?
I made two batches lately and both raise questions. The first... I tried stir-washing for the first time. The water separated out, slightly cloudy but I'm left with a thin butterscotch looking biodiesel. It's been settling for a few days, even added heat up to 165°F. No change. Any thoughts? The second... I made a batch from a new oil source. I made a 1L test batch with a titration of 5.6. Higher than what I used to but the test batch came out good. I duplicated it on a 55gal batch; I mixed for 1 hour and held at 137°F for the process. Now I have some concoction that has a watery-looking dark brown layer on top and a light brown on the bottom. No glyercine separated. When I mix with the pump on the reactor, the two layers don't want to mix together. It looks like milk and alcohol. I did a wash test, mixing the tank while pulling a sample. It looks water-soluble - no separation, no defined layers, just a consistent mixture. Any thoughts here? It's not soap...so what is it? ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/sustainablelorgbiofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (70,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] A Norwegian alchemist
Sincere thanks, Tom - for your extensive assistance. - Your questions: 1. Yes, I have succeeded with test batches using new, unused oil - not on a basis of titration (which, as I said, gives me trouble), but on a series of test batches on the same principle as Poor man's titation - circling in the correct amount of lye. 2. Yes, I have done both Jan Warnqvist test and Wash Test. I also have succeeded with test batches of WVO. They have passed both the Wash Test and the Methanol Test. - I've been following the same procedure as with new oil - with a number of batches with different amount of lye. - It works, but it takes a lot of time. - Titration: I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphthalein - but I'm having the same incomprehensible results. Is this after you made fresh titration solution? (1 g NaOH per Liter of distilled water) Is your balance accurate to tenths of a gram? Some digital scales are only accurate to whole grams. I'm concerned that your titration solution may be the problem. - Yes, this is with fresh titration solution (5 grammes NaOH in 500 ml distilled water - diluted further 1:9). - I use a 0,01 g electronic balance. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphtalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? - My failed Wash Tests: I have had both variants - too much soap between the water and BD layer, - and: Emulsion forms, and the separation fails to happen within 30 minutes. Do these Wash Test results tell whether there has been too much or too little lye - or methanol - in the reaction? - Settling time: I always use more than 8 hours, normally12 hours or more. I syphon the BD from the glycerine mix - very carefully. Conclusion so far: My main problem is the tiration. Solving that mystery woud be a breakthrough. With kind regards from a summery Oslo - my WVO melting in the sun - Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Thursday, June 05, 2008 4:12 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Sorry I'm a bit slow to respond. I'm juggling a number of projects at the moment. It is not unusual to have some problems with test batches. It is also common to achieve success and then run into problems scaling up to larger batch size. It invariably turns out to be a simple mistake that must be corrected or a simple adjustment to the process. The biggest danger is over-thinking. Let's not, for the moment, be concerned with other methods or tricks. Let's get the simplest, tried-and-true method to work, and then you can, if you like, move on to other methods. When you ultimately meet with success you will look back and say: It was all there. The instructions at JtF were all I really needed. First: 0.5L - 1.0L test batches using NEW, UNUSED veg oil. Have you done this?Did you have success? The reason for starting with new, unused veg oil is that you eliminate the need for titration. This allows you to focus on the process. If you achieve a good split, pass the wash test, and the Jan Warnqvist quality test, you are ready to move on to test batches w. used (WVO) veg oil. Success with new, unused veg oil resolves any questions about agitation, temp, quality of caustic, methanol and reaction time. You can proceed knowing that you have these variables under control. Second: 0.5L - 1.0L test batches with used (WVO) oil. Success with step one gives confidence and brings a number of variables under control. Step two (WVO) allows you to focus on titration. It also allows you to see the effect of Free Fatty Acids (FFAs), present in WVO, on soap formation, and hence, on the appearance of the wash tests. Note: (This may make sense now; will help answer one of your questions later) - Little soap should be formed when processing new, unused veg oil. What little soap is produced is due to the inevitable, though small, amount of water in the ingredients. - More soap will be produced when processing WVO due to the presence of FFAs which, in the single stage base method, are converted to soap. *** By starting with new, unused veg oil we not only avoid titration in processing the oil, we minimize soap production which can make for problems in the wash. My questions: 1. Have you succeeded with test batches using new, unused veg oil? 2. -If yes, have you done the solubility in methanol quality test (Jan W. test described at JtF), or only the wash test? You must do both. Together they form the basis for
Re: [Biofuel] A Norwegian alchemist
Ove, Sincere thanks, Tom - You are most welcome. Let's see if we can straighten out the difficulties with titration. Each ml of 0.1% titration solution contains .001 g of NaOH. Each ml of titration solution used on a ml of veg oil corresponds to a gram of the same caustic per Liter of the same veg oil. This all works fine if: Your isopropyl alcohol is neutral. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphthalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? Your isopropyl alcohol is a bit acidic. Some of your titration solution is being used to neutralize the isopropyl alcohol. This should produce higher titration values. But: (From a previous post dated 6/1/08) The first successful batch with used oil contained 2,5 grammes extra of NaOH, but the titration indicated only 0,6 grammes. Titration always gave too low values. Further: (Same 6/1/08 post) When I used a pH-paper on an oil-isopropyl alcohol solution that had turned pink, it showed 5 or 6! Phenolphthalein should not turn pink until a pH of about 8.2 It is essential that you have good phenolphthalein solution. This could be the problem as a color change at 5 or 6 would result in the low titration values you have gotten. (More titration solution would have been required to achieve the pH of 8.2 we are striving for.) ***Try adding 2 drops of phenolphthalein to 10ml of distilled water. Add titration solution drop-by-drop until it turns pink/purple. Check mix with pH paper. It should be about 8. I have tried to change the phenolphthalein - without luck. Do you mean you were unable to get a fresh supply of phenolphthalein? If you are unable to acquire reliable phenolphthalein I would be happy to mail you some phenolphthalein (powder or solution) so long as it is legal to do so. Best to You, Tom - Original Message - From: Ove Steen [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Friday, June 06, 2008 7:16 AM Subject: Re: [Biofuel] A Norwegian alchemist Sincere thanks, Tom - for your extensive assistance. - Your questions: 1. Yes, I have succeeded with test batches using new, unused oil - not on a basis of titration (which, as I said, gives me trouble), but on a series of test batches on the same principle as Poor man's titation - circling in the correct amount of lye. 2. Yes, I have done both Jan Warnqvist test and Wash Test. I also have succeeded with test batches of WVO. They have passed both the Wash Test and the Methanol Test. - I've been following the same procedure as with new oil - with a number of batches with different amount of lye. - It works, but it takes a lot of time. - Titration: I'm using the recipe of JtF: 1 ml of oil, 10 ml of isopropyl, 2 drops of phenolphthalein - but I'm having the same incomprehensible results. Is this after you made fresh titration solution? (1 g NaOH per Liter of distilled water) Is your balance accurate to tenths of a gram? Some digital scales are only accurate to whole grams. I'm concerned that your titration solution may be the problem. - Yes, this is with fresh titration solution (5 grammes NaOH in 500 ml distilled water - diluted further 1:9). - I use a 0,01 g electronic balance. Today I've been testing the isopropyl alcohol the way you told me: 10 ml isopropyl alcohol + 2 drops of phenolphtalein - then adding freshly made titration solution drop by drop. What happens, is: The solution turns barely purple on the first drop - but it doesn't stay purple. On drop no 7 it turns deeper purple, and stays purple for some time. - What does this tell? - My failed Wash Tests: I have had both variants - too much soap between the water and BD layer, - and: Emulsion forms, and the separation fails to happen within 30 minutes. Do these Wash Test results tell whether there has been too much or too little lye - or methanol - in the reaction? - Settling time: I always use more than 8 hours, normally12 hours or more. I syphon the BD from the glycerine mix - very carefully. Conclusion so far: My main problem is the tiration. Solving that mystery woud be a breakthrough. With kind regards from a summery Oslo - my WVO melting in the sun - Ove - Original Message - From: Thomas Kelly [EMAIL PROTECTED] To: sustainablelorgbiofuel@sustainablelists.org Sent: Thursday, June 05, 2008 4:12 PM Subject: Re: [Biofuel] A Norwegian alchemist Ove, Sorry I'm a bit slow to respond. I'm juggling a number of projects at the moment. It
