Re: [Biofuel] Re: A beginners titration question
Hi Fred Keith, Great Information, You got ribbons too? :-) No ribbons. My daughter might want one!! Ah, well, Fred, for her, of course, special arrangements can always be made. I hope she won't mind if it's wrapped round a bunch of roses though. All best Keith fred On 8/11/05, Keith Addison [EMAIL PROTECTED] wrote: Thanks Jan for the explanation. And Keith I am sorry that I irritated you with a dumb question, I will avoid that in the future. For heaven's sake, that's the second time! I wasn't irritated, but now I am! You got good information, do you want a red ribbon round it too? :-( Keith Addison Doug snip ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] Re: A beginners titration question
Hello Doug. Keith has made an excellent input to you questions but I felt it necessary to add some aspects of your problem: The rule no1 when taking samples is to make sure - as possible- that the sample is representative for the batch. This sounds simple, but if you are dealing with high water content together with high FFA levels you will have different titration values if sampled from the top or from the bottom. If there are detergents in the oil, this actually may help. It is a disadvantage when washing the biodiesel though. By using IPA for titration, the general idea is to have one clear phase consisting from IPA, water, KOH (or NaOH) and oil. The EN standard for determination of acid number which is likewise determined by titration strongly recommends that the amount of IPA should be increased if the solution becomes cloudy or turbid. By using methanol for titration, you are out of standard procedure. And - possibly annoying Keith - the EN requirement for a good titration is that the solution stays magenta for at least 15 seconds. Good luck to you further on ! With best regards Jan Warnqvist AGERATEC AB [EMAIL PROTECTED] + 46 554 201 89 +46 70 499 38 45 - Original Message - From: Keith Addison [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Thursday, August 11, 2005 9:38 AM Subject: [Biofuel] Re: A beginners titration question Hello Doug Hello group, I am a beginner in the conversion of WVO to BD and I have been having trouble with my titration process. On JTF there are 2 reference documents on titration which I have been using as my guide. There's more than that there about titration. However, I don't seem to get consistent results. For example, One time I will get 1.55ml and the second time I get 3.22 ml using WVO from the same batch and drawing from the same solution of NaOH and water. First is that kind of variability to be expected? No. Second I noticed in reviewing the tritration documents again, that isopropyl alcohol is specifed. But how could you not have noticed that the first time round? Everywhere is says so. I have been using the same methanol that I use in the conversion process. Prefacing this with I ain't no chemist, Is that the source of my problem? If that is the case can someone explain why the titration is done with one type of alcohol when the process is run with a different one? I also ain't no chemist, very few of us are chemists, but we can learn, and do. I can't give you a technical comparison of the effects of different alcohols, but why depart from established practice when you're just starting? It doesn't make a lot of sense anyway, titration and processing have different purposes, with titration you're only finding out how much acid will have to be neutralised, not processing the WVO. The result of the titration is applied to the subsequent processing in the form of the amount of lye required, not the kind of alcohol to use. If you assume that the two different processes should use the same alcohol then why don't you also assume that they should use it in the same proportions? - ie 10 litres of 99%+ isopropyl alcohol per one litre of WVO to be processed? Anyway, it is possible to use isopropyl alcohol to make biodiesel, called branched-alkyl esters, which have the advantage of much improved cold-weather properties. There's discussion of this in the list archives, using either isopropyl alcohol or butanol. But it's not for homebrewers, though many have tried - it's laboratory-level stuff, patented but not used, nobody is using these techniques yet AFAIK. Also I seem to be having difficulty keeping the WVO and alcohol mixed during the titration process, which would be what I would attribute to the variation in the results. I don't think so. I have been carrying out the titration in a test tube and shaking it after each drop, but the oil still seems to settle out. Stirring is better. Did you warm the mixture first (and the 0.1% NaOH solution)? Use something wider than a test tube that you can stir. And even when they are mixed it is a cloudy white solution, not clear as the JTF documents indicate. They do not indicate that. What they say is that it should be clear (thoroughly mixed) BEFORE you start adding the 0.1% NaOH solution. Warm the beaker gently by standing it in some hot water, stir until all the oil dissolves in the alcohol and turns clear. Add 2 drops of phenolphthalein solution. Using a graduated syringe, add 0.1% lye solution drop by drop to the oil-alcohol-phenolphthalein solution, stirring all the time, until the solution starts to turn pink and stays that way for 10 seconds. ... Biodiesel from waste oil http://journeytoforever.org/biodiesel_make.html#biodwvo Dissolve 1 gram of lye in 1 liter of distilled or de-ionized water (0.1% w/v lye solution). In a smaller beaker, dissolve 1 ml of dewatered WVO oil in 10 ml of pure isopropyl alcohol. Warm
Re: [Biofuel] Re: A beginners titration question
Hello Jan Hello Doug. Keith has made an excellent input to you questions but I felt it necessary to add some aspects of your problem: The rule no1 when taking samples is to make sure - as possible- that the sample is representative for the batch. This sounds simple, but if you are dealing with high water content together with high FFA levels you will have different titration values if sampled from the top or from the bottom. If there are detergents in the oil, this actually may help. It is a disadvantage when washing the biodiesel though. Good advice. Another little-noticed problem is transferring sample-test results to the full-sized reactor, with its different rate of agitation, different shape, different temperature maintenance and so on. Trial and error, more or less, until you get the best results. Bracketed tests help fine-tune it at each stage, perhaps followed by wash tests of each sample result: Poor man's titration http://journeytoforever.org/biodiesel_make2.html#poor Quality testing http://journeytoforever.org/biodiesel_vehicle.html#quality By using IPA for titration, the general idea is to have one clear phase consisting from IPA, water, KOH (or NaOH) and oil. The EN standard for determination of acid number which is likewise determined by titration strongly recommends that the amount of IPA should be increased if the solution becomes cloudy or turbid. If you stir it vigorously it'll be fine. By using methanol for titration, you are out of standard procedure. And - possibly annoying Keith :-) I might argue Jan but I seldom get annoyed. - the EN requirement for a good titration is that the solution stays magenta for at least 15 seconds. That's at one end of the scale, at the opposite end is that it starts to go pink (before magenta) and stays that way for 10 seconds. I'd leave it to individuals to decide which is best for them, again bracketed tests followed by wash tests of each sample result will help. Best Keith Good luck to you further on ! With best regards Jan Warnqvist AGERATEC AB [EMAIL PROTECTED] + 46 554 201 89 +46 70 499 38 45 - Original Message - From: Keith Addison [EMAIL PROTECTED] To: biofuel@sustainablelists.org Sent: Thursday, August 11, 2005 9:38 AM Subject: [Biofuel] Re: A beginners titration question Hello Doug Hello group, I am a beginner in the conversion of WVO to BD and I have been having trouble with my titration process. On JTF there are 2 reference documents on titration which I have been using as my guide. There's more than that there about titration. However, I don't seem to get consistent results. For example, One time I will get 1.55ml and the second time I get 3.22 ml using WVO from the same batch and drawing from the same solution of NaOH and water. First is that kind of variability to be expected? No. Second I noticed in reviewing the tritration documents again, that isopropyl alcohol is specifed. But how could you not have noticed that the first time round? Everywhere is says so. I have been using the same methanol that I use in the conversion process. Prefacing this with I ain't no chemist, Is that the source of my problem? If that is the case can someone explain why the titration is done with one type of alcohol when the process is run with a different one? I also ain't no chemist, very few of us are chemists, but we can learn, and do. I can't give you a technical comparison of the effects of different alcohols, but why depart from established practice when you're just starting? It doesn't make a lot of sense anyway, titration and processing have different purposes, with titration you're only finding out how much acid will have to be neutralised, not processing the WVO. The result of the titration is applied to the subsequent processing in the form of the amount of lye required, not the kind of alcohol to use. If you assume that the two different processes should use the same alcohol then why don't you also assume that they should use it in the same proportions? - ie 10 litres of 99%+ isopropyl alcohol per one litre of WVO to be processed? Anyway, it is possible to use isopropyl alcohol to make biodiesel, called branched-alkyl esters, which have the advantage of much improved cold-weather properties. There's discussion of this in the list archives, using either isopropyl alcohol or butanol. But it's not for homebrewers, though many have tried - it's laboratory-level stuff, patented but not used, nobody is using these techniques yet AFAIK. Also I seem to be having difficulty keeping the WVO and alcohol mixed during the titration process, which would be what I would attribute to the variation in the results. I don't think so. I have been carrying out the titration in a test tube and shaking it after each drop, but the oil still seems to settle out. Stirring is better. Did you warm the mixture first (and the 0.1% NaOH solution)? Use something
Re: [Biofuel] Re: A beginners titration question
Keith, Great Information, You got ribbons too? My daughter might want one!! fred On 8/11/05, Keith Addison [EMAIL PROTECTED] wrote: Thanks Jan for the explanation. And Keith I am sorry that I irritated you with a dumb question, I will avoid that in the future. For heaven's sake, that's the second time! I wasn't irritated, but now I am! You got good information, do you want a red ribbon round it too? :-( Keith Addison Doug Hello Doug Hello group, I am a beginner in the conversion of WVO to BD and I have been having trouble with my titration process. On JTF there are 2 reference documents on titration which I have been using as my guide. There's more than that there about titration. However, I don't seem to get consistent results. For example, One time I will get 1.55ml and the second time I get 3.22 ml using WVO from the same batch and drawing from the same solution of NaOH and water. First is that kind of variability to be expected? No. Second I noticed in reviewing the tritration documents again, that isopropyl alcohol is specifed. But how could you not have noticed that the first time round? Everywhere is says so. I have been using the same methanol that I use in the conversion process. Prefacing this with I ain't no chemist, Is that the source of my problem? If that is the case can someone explain why the titration is done with one type of alcohol when the process is run with a different one? I also ain't no chemist, very few of us are chemists, but we can learn, and do. I can't give you a technical comparison of the effects of different alcohols, but why depart from established practice when you're just starting? It doesn't make a lot of sense anyway, titration and processing have different purposes, with titration you're only finding out how much acid will have to be neutralised, not processing the WVO. The result of the titration is applied to the subsequent processing in the form of the amount of lye required, not the kind of alcohol to use. If you assume that the two different processes should use the same alcohol then why don't you also assume that they should use it in the same proportions? - ie 10 litres of 99%+ isopropyl alcohol per one litre of WVO to be processed? Anyway, it is possible to use isopropyl alcohol to make biodiesel, called branched-alkyl esters, which have the advantage of much improved cold-weather properties. There's discussion of this in the list archives, using either isopropyl alcohol or butanol. But it's not for homebrewers, though many have tried - it's laboratory-level stuff, patented but not used, nobody is using these techniques yet AFAIK. Also I seem to be having difficulty keeping the WVO and alcohol mixed during the titration process, which would be what I would attribute to the variation in the results. I don't think so. I have been carrying out the titration in a test tube and shaking it after each drop, but the oil still seems to settle out. Stirring is better. Did you warm the mixture first (and the 0.1% NaOH solution)? Use something wider than a test tube that you can stir. And even when they are mixed it is a cloudy white solution, not clear as the JTF documents indicate. They do not indicate that. What they say is that it should be clear (thoroughly mixed) BEFORE you start adding the 0.1% NaOH solution. Warm the beaker gently by standing it in some hot water, stir until all the oil dissolves in the alcohol and turns clear. Add 2 drops of phenolphthalein solution. Using a graduated syringe, add 0.1% lye solution drop by drop to the oil-alcohol-phenolphthalein solution, stirring all the time, until the solution starts to turn pink and stays that way for 10 seconds. ... Biodiesel from waste oil http://journeytoforever.org/biodiesel_make.html#biodwvo Dissolve 1 gram of lye in 1 liter of distilled or de-ionized water (0.1% w/v lye solution). In a smaller beaker, dissolve 1 ml of dewatered WVO oil in 10 ml of pure isopropyl alcohol. Warm the beaker gently by standing it in some hot water, stir until all the oil dissolves in the alcohol and the mixture turns clear. Add 2 drops of phenolphthalein solution. Using a graduated syringe, add the 0.1% lye solution drop by drop to the oil-alcohol-phenolphthalein solution, stirring all the time, until the solution stays pink (actually magenta) for 10 seconds. ... Basic titration http://journeytoforever.org/biodiesel_make2.html#titrate Instead of the usual 1 ml of oil and 10 ml of isopropyl alcohol, mix 4 ml of oil in 40 ml of isopropyl alcohol in a glass beaker. Warm the mixture gently by standing the beaker in hot water, stir until all the oil disperses and it becomes a clear mixture. Then titrate as usual, measuring milliliters of stock solution used. ... Better titration http://journeytoforever.org/biodiesel_make2.html#bettertitrate Mix 10 milliliters of isopropyl
