pump mixing, was: [Biofuel] more on the quality test
As for the sample, it's not surprising that there was incomplete conversion. Pumps don't provide the interaction needed to keep a tank's contents in continual bedlam, at least not the small pump mentioned and even more doubtful based upon the short duration it was activated. They may mix, but outside the main flowstream there is little agitation. I would have suggested that the reaction time be not less than six hours even before seeing the post. In an environment where feedstock isn't backing up on the dock, there's no need to try and rush. are you suggesting that pump mixing in general is a bad idea? it's a good thing you mention this now as I am starting to collect materials for my processor which was going to be based on the touchless/luc's/jtf 90L plus some minor modifications that relate to electronic control (I am a geek I can't help myself, if I can program a microprocessor to watch the clock and flip a switch why do it myself :) I would like people's thoughts in general about pump mixing, I wanted to use the hot water heater tank because I just scored an 80 gal unit that is perfectly functional and it is well insulated so it will take less energy to heat but if prop mixing is the way to go I could change my course (I could use the water heater for a preheat tank for example). We use 16-24 hour reaction times in a 400 gallon reactor for two primary reasons. The first is that we have no desire (yet) to start leaning the process out and begin bumping into problems. I had already been considering significantly longer mixing times, my last batch I mixed to 2 hours instead of the 1.5 that I had been doing previously and I didn't have a noticeable change in yield although I didn't make any attempt to really measure that accurately (just by the mark on the mason jar). I assume that this won't make up for poor temperature control but it will make up for less good mixing, does anyone have any data to back this up or dispute it? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: pump mixing, was: [Biofuel] more on the quality test
I'm not saying that pump mixing is a bad idea. I am saying that there are more efficient and thorough ways to mix. The clear water pump that so many are opting to use might be okay for a five or ten gallon volume, but not much bigger. Perhaps it might work on larger volumes if it were installed so that the outlet stream flowed slightly less than parallel to the ground and at an high-oblique angle to the side of a round-tank reactor so that a vortex could be created. That could be done by installing a maleable copper tube inside the tank to get the right angle of flow. But still, the current from the outlet stream doesn't extend over a very large surface area, leaving much of a tank's contents more or less idle in comparison to prop agitation. My suggestion would be that if a person is dead set on a pump and is running a 30-50 gallon reactor, they look at either prop agitation or larger pumps. Some reasonably priced, high volume pumps can be found at http://www.surpluscenter.com/sort.asp?UID=2005010414190186catname=waterkeyword=WPCA If a person uses prop agitation, they would still want to use a TEFC motor. A non-pressure rated, nylon, shaft seal would work reasonably well for vapor containment, providing that a sufficiently sized vent (leading to a condensor or outside the work area, preferably the former) was built into the reactor top. That seal could be as simple as a secured, flexible, 10 mil, sheet of nylon with a hole diameter slightly less than the prop shaft diameter. Pressure rated seals can be acquired through almost any bearing/packing supply haus. Todd Sweairngen - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Monday, January 03, 2005 5:41 PM Subject: pump mixing, was: [Biofuel] more on the quality test Todd, As for the sample, it's not surprising that there was incomplete conversion. Pumps don't provide the interaction needed to keep a tank's contents in continual bedlam, at least not the small pump mentioned and even more doubtful based upon the short duration it was activated. They may mix, but outside the main flowstream there is little agitation. I would have suggested that the reaction time be not less than six hours even before seeing the post. In an environment where feedstock isn't backing up on the dock, there's no need to try and rush. are you suggesting that pump mixing in general is a bad idea? it's a good thing you mention this now as I am starting to collect materials for my processor which was going to be based on the touchless/luc's/jtf 90L plus some minor modifications that relate to electronic control (I am a geek I can't help myself, if I can program a microprocessor to watch the clock and flip a switch why do it myself :) I would like people's thoughts in general about pump mixing, I wanted to use the hot water heater tank because I just scored an 80 gal unit that is perfectly functional and it is well insulated so it will take less energy to heat but if prop mixing is the way to go I could change my course (I could use the water heater for a preheat tank for example). We use 16-24 hour reaction times in a 400 gallon reactor for two primary reasons. The first is that we have no desire (yet) to start leaning the process out and begin bumping into problems. I had already been considering significantly longer mixing times, my last batch I mixed to 2 hours instead of the 1.5 that I had been doing previously and I didn't have a noticeable change in yield although I didn't make any attempt to really measure that accurately (just by the mark on the mason jar). I assume that this won't make up for poor temperature control but it will make up for less good mixing, does anyone have any data to back this up or dispute it? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: pump mixing, was: [Biofuel] more on the quality test
I use a 1 clear water pump but only do 80 liter batches and process for two hours minimum. I have not had any significant problems with incomplete reactions attributed to this, however if I were to get into larger batches it only seems right to increase the processing time. Larger volumes will require a bigger pump also. The clear water pump is fine for small batches like what I do, but if you are goping for larger then a stronger pump will be needed. 80 gals isn't going to make it on the one inch pump that I use right now. I am now in the process of expanding the system though. I have a secondary 200 liter drum and stand fopr it already and have begun working on it. I will stil process 80 liters per batch, but make two at a time and settle the second in the other drum and the first in the reactor itself. Luc - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Monday, January 03, 2005 5:41 PM Subject: pump mixing, was: [Biofuel] more on the quality test Todd, As for the sample, it's not surprising that there was incomplete conversion. Pumps don't provide the interaction needed to keep a tank's contents in continual bedlam, at least not the small pump mentioned and even more doubtful based upon the short duration it was activated. They may mix, but outside the main flowstream there is little agitation. I would have suggested that the reaction time be not less than six hours even before seeing the post. In an environment where feedstock isn't backing up on the dock, there's no need to try and rush. are you suggesting that pump mixing in general is a bad idea? it's a good thing you mention this now as I am starting to collect materials for my processor which was going to be based on the touchless/luc's/jtf 90L plus some minor modifications that relate to electronic control (I am a geek I can't help myself, if I can program a microprocessor to watch the clock and flip a switch why do it myself :) I would like people's thoughts in general about pump mixing, I wanted to use the hot water heater tank because I just scored an 80 gal unit that is perfectly functional and it is well insulated so it will take less energy to heat but if prop mixing is the way to go I could change my course (I could use the water heater for a preheat tank for example). We use 16-24 hour reaction times in a 400 gallon reactor for two primary reasons. The first is that we have no desire (yet) to start leaning the process out and begin bumping into problems. I had already been considering significantly longer mixing times, my last batch I mixed to 2 hours instead of the 1.5 that I had been doing previously and I didn't have a noticeable change in yield although I didn't make any attempt to really measure that accurately (just by the mark on the mason jar). I assume that this won't make up for poor temperature control but it will make up for less good mixing, does anyone have any data to back this up or dispute it? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
Appal Energy wrote: Well, I got my report back from Magellan Midstream. My sample tested as follows: That was rather quick.. Glad Ms. Alovert was able to direct you to a place that can give you answers quickly, as well as precisely. Which sample did you submit? this was quoted from the link right below it as indicated by the quote and /quote around it, I apologize if that is not clear. 0.002 mass% Free Glycerin 0.940 mass% Monoglyceride 1.084 mass% Diglyceride 3.911 mass% Triglyceride 0.815 mass% Tot. Glycerin And just what is it that you see wrong with these numbers? this is an example of fuel without high enough mono or di glycerides to fail the wash test but high enough triglycerides to push it out of spec. ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
And just what is it that you see wrong with these numbers? this is an example of fuel without high enough mono or di glycerides to fail the wash test but high enough triglycerides to push it out of spec. I ddin't realize the sample you mentioned was from someone else's venture. I tend to veer away from Infopop for a number of reasons. One is all the collaborative guesswork. The other is all the manufactured credentials of so many of the members there. One month someone's just becoming familiar with biodiesel and six months to two years later they're renowned or a chemist or have 10 years of bidiesel experience. Combine so many variables/free-radicals and it only seems prudent to move in a manner where results are a bit more verifiable. As for the sample, it's not surprising that there was incomplete conversion. Pumps don't provide the interaction needed to keep a tank's contents in continual bedlam, at least not the small pump mentioned and even more doubtful based upon the short duration it was activated. They may mix, but outside the main flowstream there is little agitation. I would have suggested that the reaction time be not less than six hours even before seeing the post. In an environment where feedstock isn't backing up on the dock, there's no need to try and rush. We use 16-24 hour reaction times in a 400 gallon reactor for two primary reasons. The first is that we have no desire (yet) to start leaning the process out and begin bumping into problems. The second is that the reactor is an adapted horizontal dairy tank with a twin-prop (one 4 and one 6, with 3/4 hp drive at 1,200 rpm), vertical mixer. Even with the extra agitation, the farther reaches of the horizontal tank tend to be more calm than the center, unlike the vortex that would form in a vertical tank (even with baffles). The second thing I would have suggested is that well before submitting a sample for testing, a Po' Man's Titration be conducted, as well as side-by-side wash tests of each sample from the same set of bracket titrations to better gain an understanding of what the effects of different levels of caustic are. I've made the recommendation before that anyone who's made but one successful liter of fuel conduct a one or two bracket tests (varying ranges or a larger number of samples), preferably before moving on to bigger game. The difference of 1/2 gram of caustic below or above minimum per liter of feedstock can yield some very quantifiable difference between samples. In the wash it can mean a difference between a clean separation in 30 seconds or less and a slightly milky but thin layer that appears to be complete separation . Todd Swearingen - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Sunday, January 02, 2005 12:48 AM Subject: Re: [Biofuel] more on the quality test Appal Energy wrote: Well, I got my report back from Magellan Midstream. My sample tested as follows: That was rather quick.. Glad Ms. Alovert was able to direct you to a place that can give you answers quickly, as well as precisely. Which sample did you submit? this was quoted from the link right below it as indicated by the quote and /quote around it, I apologize if that is not clear. 0.002 mass% Free Glycerin 0.940 mass% Monoglyceride 1.084 mass% Diglyceride 3.911 mass% Triglyceride 0.815 mass% Tot. Glycerin And just what is it that you see wrong with these numbers? this is an example of fuel without high enough mono or di glycerides to fail the wash test but high enough triglycerides to push it out of spec. ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
follows: That was rather quick.. Glad Ms. Alovert was able to direct you to a place that can give you answers quickly, as well as precisely. Which sample did you submit? 0.002 mass% Free Glycerin 0.940 mass% Monoglyceride 1.084 mass% Diglyceride 3.911 mass% Triglyceride 0.815 mass% Tot. Glycerin And just what is it that you see wrong with these numbers? priorities at present rank figuring out what is going on Answer: You're not getting a complete reaction. Question: Why? Answer: Insufficient turnover rate? Insufficient reaction time? Insufficient catalyst? Insufficient alcohol? Insufficient reaction temperature? If you look back over your notes and your general process, you should be able to deduce where your shortfall was. if you have soap but no mono, di, or triglycerides will anything drop out? Little to nothing. Whatever soap existed prior to introducing new methoxide was in suspension. Addition of new methoxide will slightly lessen the specific gravity of the total volume, which might permit some visible settling. As well, introducing more catalyst will crack a few molecules of fuel and convert them to soap. But overall there should be nothing of note. You may wish to conduct a test to see how miscible MeOH is in biodiesel. It might surprise you relative to any volume you may expect to see drop out upon reprocessing. not looking for outs. if the instructions on the wash test had said if you have really high quality fuel it will settle in 4 minutes whereas passable fuel will settle in 30 minutes or less I would have personally made the decision to work on the 4 minute fuel (I am kind of picky and I like my car a lot). Common sense should have told you that up front, all things being equal. I would presently be disappointed with anything that settled in longer than 5 minutes at 70 degrees (which disagrees with the instructions). You're entitled to disagree with whatever you wish. But you still haven't established beyond the first doubt that what you read isn't applicable to well processed fuel, even though you're implying such. I understand that the people prodding you behind the scenes would like to take issue with anything and everything they can. But let's be upfront and honest about it and stick to the facts, not supposition, eh? Todd Swearingen - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Friday, December 31, 2004 12:37 AM Subject: Re: [Biofuel] more on the quality test Appal Energy wrote: If you've got triglycerides remaining you'll also have the emulsifying mono- and di-glycerides, primary emulsifiers. If you've got no emulsifiers present, then you're going to be very hard pressed to find any registerable amount of triglycerides. It's really an either/or scenario. This is where a wash test is a fair indicator. If emulsion forms using water of room temp, presuming sufficient settling time has been conducted (and better still if the reaction was a/b), then you know you've got incompletely reacted mono- and di-glycerides. Whether or not you know the molecular ratio of each, much less that of any tri-glycerides is relatively a non-issue. http://biodiesel.infopop.cc/eve/ubb.x?a=tpcs=447609751f=719605551m=926101095 quote Well, I got my report back from Magellan Midstream. My sample tested as follows: 0.002 mass% Free Glycerin 0.940 mass% Monoglyceride 1.084 mass% Diglyceride 3.911 mass% Triglyceride 0.815 mass% Tot. Glycerin /quote I am less concerned with altering the process to achieve less soap (it seems to produce little enough as it is, provided that you use the right amount of lye) than I am with finding a method to tell the difference between an underreacted batch and a soapy batch, Well, if that's the case, I'd have to say that you've got your priorities out of order. priorities at present rank figuring out what is going on highest of all so when I start doing this for real I really know :) the answer is reprocess a sample of the batch that failed and look for glyc to drop out, if it dosen't you have soap problems, That's not true. Soap drops with the glyc. If nothing drops then you have no problem. if you have soap but no mono, di, or triglycerides will anything drop out? if it does you have underreacted your batch. this may also be my test for triglycerides. No. It just tells you that you had an underreacted batch, not the ratios of underreacted components. yes, but if you pass the wash test and you still get something dropping out then that would indicate triglycerides as they don't emulsify. I understand, but perhaps having a sense of really great fuel will separate within 4 minutes at 70 degrees wheras less good but passable fuels will separate in 10 or more minutes with the outside limit of pasability being 30 minutes would be helpful. You want a green light so that you can run incompleted fuel through your
Re: [Biofuel] more on the quality test
I will keep a small sample and see if I can get it tested, will post the results. Peter At 10:12 AM 30/12/2004 -0500, you wrote: Peter, Interesting as to the precipitate you achieved. You might wish to dry it and test its properties. A safe bet is that it's a flocculent of multiple constituents, as non-water soluble calcium soaps by themselves have specific gravities less than water and would float in water rather than settle. See http://www.gogenchem.com/calcium/NCh14.html We've been eying CaCl2 as a less expensive option for treatment of wash water prior to its release as graywater. Question for us is whether it's more environmentally friendly than magnesium sulfate. Based upon your experience, it might be a fair idea to keep calcium chloride in mind as an emulsion breaker. The compound has been mentioned before in conversation on this list, but I believe it was more as a drying agent in other applications. It might also be a good idea that some honest labwork be conducted to see exactly what benefits (if any) such a measure can achieve in a less than marginal fuel situation. It's possible that under the right conditions calcium can not only break an emulsion but convert some residual glycerides from incomplete reactions to soaps that can be removed. But I wouldn't recommend that anyone who reads this go off half-cocked and start preaching it as a one size fits all solution to production problems until some legitimate labwork could confirm its benefits and/or disbenefits. As for whether or not calcium chloride could become a contaminant? It is water soluble and should wash out. The same can be said for potassium and/or sodium chloride, which would become present if the CaCl2 actually converts some or all of the water soluble soaps to insoluble calcium grease (lime grease). Todd Swearingen - Original Message - From: Peter Harves [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Thursday, December 30, 2004 5:52 AM Subject: Re: [Biofuel] more on the quality test Todd, Thank you , I was most interested in your post as I am new to making Bio (450lts so far) I had a bad batch which was like milk, I put it aside to let it settle over a week, it did but very little. I bought a new aerator and I think I agitated the mix to much!!! I am a potter and use all sorts of chemicals for my glazes so I thought I would try some to separate the glob. I used Calcium Chloride about 40 ml in a 90ltr batch , the reaction was interesting, both started to separate leaving the soaps in a curdled layer at the bottom . I decanted the clear bio to my wash vessel, I have now washed it 2x and will wash again it is very clear now. Question-- calcium chloride is water soluble, that's why I want to wash it well, but would it do any harm to the engine if there were traces left in the fuel for some reason or other??? if you don't know the answer maybe somebody out there might !. I know this is not the way to make Bio but I didn't want to throw out the batch and I guess we all like to experiment . Peter. ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
Appal Energy wrote: If you've got triglycerides remaining you'll also have the emulsifying mono- and di-glycerides, primary emulsifiers. If you've got no emulsifiers present, then you're going to be very hard pressed to find any registerable amount of triglycerides. It's really an either/or scenario. This is where a wash test is a fair indicator. If emulsion forms using water of room temp, presuming sufficient settling time has been conducted (and better still if the reaction was a/b), then you know you've got incompletely reacted mono- and di-glycerides. Whether or not you know the molecular ratio of each, much less that of any tri-glycerides is relatively a non-issue. http://biodiesel.infopop.cc/eve/ubb.x?a=tpcs=447609751f=719605551m=926101095 quote Well, I got my report back from Magellan Midstream. My sample tested as follows: 0.002 mass% Free Glycerin 0.940 mass% Monoglyceride 1.084 mass% Diglyceride 3.911 mass% Triglyceride 0.815 mass% Tot. Glycerin /quote I am less concerned with altering the process to achieve less soap (it seems to produce little enough as it is, provided that you use the right amount of lye) than I am with finding a method to tell the difference between an underreacted batch and a soapy batch, Well, if that's the case, I'd have to say that you've got your priorities out of order. priorities at present rank figuring out what is going on highest of all so when I start doing this for real I really know :) the answer is reprocess a sample of the batch that failed and look for glyc to drop out, if it dosen't you have soap problems, That's not true. Soap drops with the glyc. If nothing drops then you have no problem. if you have soap but no mono, di, or triglycerides will anything drop out? if it does you have underreacted your batch. this may also be my test for triglycerides. No. It just tells you that you had an underreacted batch, not the ratios of underreacted components. yes, but if you pass the wash test and you still get something dropping out then that would indicate triglycerides as they don't emulsify. I understand, but perhaps having a sense of really great fuel will separate within 4 minutes at 70 degrees wheras less good but passable fuels will separate in 10 or more minutes with the outside limit of pasability being 30 minutes would be helpful. You want a green light so that you can run incompleted fuel through your engine? Why not strive for completed reactions rather than outs? not looking for outs. if the instructions on the wash test had said if you have really high quality fuel it will settle in 4 minutes whereas passable fuel will settle in 30 minutes or less I would have personally made the decision to work on the 4 minute fuel (I am kind of picky and I like my car a lot). as it was noted in my previous message I attained 4 minute fuel, if my fuel had been 27 minute fuel, based on the posted instructions I would have said cool, well within spec, wash pour in tank and drive on based on my current understanding I would presently be disappointed with anything that settled in longer than 5 minutes at 70 degrees (which disagrees with the instructions). A biodieseler's biggest concerns are getting all the methanol, soap and catalyst out of the fuel at present my biggest concern is knowing that I have satisfied those concerns :) ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
as an incomplete reaction. People running SVO or WVO don't run into problems derived from soap, emulsion, residual catalyst or residual methanol. Which means that a biodieseler really needs to possess an understanding of how to keep their meddling from becoming problems in the first place - which means stop making soap, stop any practice that lends to incomplete reactions and get a cleanly washed product. It's really that simple. Todd Swearingen A biodieseler's biggest concerns are getting all the methanol, soap and catalyst out of the fuel - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Wednesday, December 29, 2004 10:21 AM Subject: Re: [Biofuel] more on the quality test Todd, Thanks for the responses. lots of good information, more questions follow. I understand that I sound like a little kid going why to everything you say but I really want to understand what I am doing here so that I can be a shining example of the products of the homebrew community and all it has to offer and not be an example of what can go wrong with homebrewing (this seems to be important for furthering the cause in general which is important to me). Appal Energy wrote: John, You prepared a 4 liter batch from which you pulled both wash samples. Yes? correct Your only variable was temperature of the wash water. Yes? correct You point out that the warmer sample separated well and the colder one not. Yes? that does seem to be the case. further it could be pointed out that (from the previous thread on this one) that 150mL samples do in fact separate much beter than 4mL ones as you suggested. So why did you dispose of the cooler sample prior to letting your experiment go one step further by allowing it to warm to the same degree as your warm sample was and then observe? In theory the end result would be the same, with the emulsion breaking and a quick settling time after re-agitating. it will never reach the 70 degrees that the other was at when it seperated because ambient temprature was 55 degrees. I let it go until it was clear that it had failed the quality test (per the instructions it should settle within 30 minutes, I gave it 40) if you would like I can leave a sample sit for a while and see if it ever seperates but I do not believe that it will in my environment (that's how I got here I had some failures sitting on the window sill waiting to separate for weeks at a time and the never really got there). I could also try setting it in a bath of 70 degree water for a while and see what happens. in that case it will probably settle out as normal (unless emulsion has some sort of inertia once formed that causes it to require more energy to break than it needed to be avoided in the first place). If your sampling was conducted to determine the effects of different wash temperatures, then you're asking the wrong questions. my testing was for temprature as a variable, these are other questions that I have yet to answer in my overall quest for homebrew quality testing procedures that will ensure that I have good enough fuel for my 2000 TDI. replacing injectors and injector pumps is expensive :) But to answer them: Testing for triglycerides would be rather unneccessary. If they are present there would also be mono- and di-glycerides and you'd know something was quite amiss when you achieved heavy emulsion in a wash. somone on the yahoo groups list (can't find the message right now, I will post a link when I do) posted results of lab tests that showed low mono or di glycerides but a high level of triglycerides. I admittadly don't understand the chemistry well enough to know why that would happen (or even if it could). perhaps really bad stirring such that part of the fluid volume never became involved in the reaction (is that possible?). As well, triglycerides don't appreciably emulsify as do mono- and di-glycerides. which is specifically why I am intarested in a test for them. suggestions that I am barking up the wrong tree are welcome :) Best method to reduce any concerns of soap formation is an acid esterification, followed by transesterification. The esterification converts to biodiesel what normally would become soap, in turn putting an end to concerns about excess soap. Once soap is almost completely eliminated from the equation through esterification and sufficient settling, unconverted glycerides by and large become the only emulsification variable. I am less concerned with altering the process to achieve less soap (it seems to produce little enough as it is, provided that you use the right amount of lye) than I am with finding a method to tell the difference between an underreacted batch and a soapy batch, something like soap emulsifies BD into the water and you get a larger amount of water after settling wheras underreacted emulsifies into the BD so you get a larger top layer
[Biofuel] more on the quality test
before testing my fuel was settled for 7 days until it was crystal clear and light yellow in color. after 24-48 hours it seemed to settle completely but it was still hazy, this went away entirely after the full 7 days. there was no appreciable increase in the volume of the glyc layer after the initial settling period. ambient temp is 55 degrees. all samples were prepared with normal city water from my tap (I don't think it is hard but there is certainly stuff in it from treatment, like chlorine for example). glassware used in measuring the samples is accurate to .24mL at 150mL (per labeling etched in the glassware). all measurements are read from the bottom of the meniscus. samples were added to a small ball jar (about 450mL volume) and then shaken for 10 seconds fairly violently. at 70 degrees F 150mL sample separated in 4m 10s, it was a celan seperation with absolutly no emulsion. there was some haze in the biodiesel like it looks when I start to wash, it goes sort of milky yellow with lots of tiny little bubbles, this will become crystal clear and even lighter yellow than it began if allowed to settle for a while (usually a day or two). at 40 degrees F 150mL sample separated in 12m 4s, there was gunk in emulsion in the FAME on top that never settled out, after about seven minutes it had separated into 60/40 (the 60 being BD) with lots of emulsion in the biodiesel layer, this emulsion never really broke but it reached about 55/45 by the 12m 4s point at which point it was as complete as it got within the 40m before I disposed of it. I don't think that I would say this passed because of the junk in the top layer and also because it never really came back to 50/50. some questions remain: this test clearly tests for three things: soap, monoglycerides, and diglycerides. how can we test for triglycerides (really incomplete reaction)? if we look at the results and say this didn't pass we should have some path for figuring out why. what methods can be used to tell the difference between excess soap and unreacted mono and di glycerides? do we learn anything from the separation time itself on a passing batch? is 4m fuel better than 10m fuel? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
You prepared a 4 liter batch from which you pulled both wash samples. Yes? Your only variable was temperature of the wash water. Yes? You point out that the warmer sample separated well and the colder one not. Yes? So why did you dispose of the cooler sample prior to letting your experiment go one step further by allowing it to warm to the same degree as your warm sample was and then observe? In theory the end result would be the same, with the emulsion breaking and a quick settling time after re-agitating. If your sampling was conducted to determine the effects of different wash temperatures, then you're asking the wrong questions. But to answer them: Testing for triglycerides would be rather unneccessary. If they are present there would also be mono- and di-glycerides and you'd know something was quite amiss when you achieved heavy emulsion in a wash. As well, triglycerides don't appreciably emulsify as do mono- and di-glycerides. Best method to reduce any concerns of soap formation is an acid esterification, followed by transesterification. The esterification converts to biodiesel what normally would become soap, in turn putting an end to concerns about excess soap. Once soap is almost completely eliminated from the equation through esterification and sufficient settling, unconverted glycerides by and large become the only emulsification variable. Yes. 4m fuel is better than 10m fuel if everything else is perfectly equal. But you can't say the same thing when you throw in variables. Todd Swearingen - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Wednesday, December 29, 2004 1:37 AM Subject: [Biofuel] more on the quality test I have completed my testing with 150mL from my 4L batch. before testing my fuel was settled for 7 days until it was crystal clear and light yellow in color. after 24-48 hours it seemed to settle completely but it was still hazy, this went away entirely after the full 7 days. there was no appreciable increase in the volume of the glyc layer after the initial settling period. ambient temp is 55 degrees. all samples were prepared with normal city water from my tap (I don't think it is hard but there is certainly stuff in it from treatment, like chlorine for example). glassware used in measuring the samples is accurate to .24mL at 150mL (per labeling etched in the glassware). all measurements are read from the bottom of the meniscus. samples were added to a small ball jar (about 450mL volume) and then shaken for 10 seconds fairly violently. at 70 degrees F 150mL sample separated in 4m 10s, it was a celan seperation with absolutly no emulsion. there was some haze in the biodiesel like it looks when I start to wash, it goes sort of milky yellow with lots of tiny little bubbles, this will become crystal clear and even lighter yellow than it began if allowed to settle for a while (usually a day or two). at 40 degrees F 150mL sample separated in 12m 4s, there was gunk in emulsion in the FAME on top that never settled out, after about seven minutes it had separated into 60/40 (the 60 being BD) with lots of emulsion in the biodiesel layer, this emulsion never really broke but it reached about 55/45 by the 12m 4s point at which point it was as complete as it got within the 40m before I disposed of it. I don't think that I would say this passed because of the junk in the top layer and also because it never really came back to 50/50. some questions remain: this test clearly tests for three things: soap, monoglycerides, and diglycerides. how can we test for triglycerides (really incomplete reaction)? if we look at the results and say this didn't pass we should have some path for figuring out why. what methods can be used to tell the difference between excess soap and unreacted mono and di glycerides? do we learn anything from the separation time itself on a passing batch? is 4m fuel better than 10m fuel? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
fuel will separate within 4 minutes at 70 degrees wheras less good but passable fuels will separate in 10 or more minutes with the outside limit of pasability being 30 minutes would be helpful. again, thanks for your response! John Guttridge Todd Swearingen - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Wednesday, December 29, 2004 1:37 AM Subject: [Biofuel] more on the quality test I have completed my testing with 150mL from my 4L batch. before testing my fuel was settled for 7 days until it was crystal clear and light yellow in color. after 24-48 hours it seemed to settle completely but it was still hazy, this went away entirely after the full 7 days. there was no appreciable increase in the volume of the glyc layer after the initial settling period. ambient temp is 55 degrees. all samples were prepared with normal city water from my tap (I don't think it is hard but there is certainly stuff in it from treatment, like chlorine for example). glassware used in measuring the samples is accurate to .24mL at 150mL (per labeling etched in the glassware). all measurements are read from the bottom of the meniscus. samples were added to a small ball jar (about 450mL volume) and then shaken for 10 seconds fairly violently. at 70 degrees F 150mL sample separated in 4m 10s, it was a celan seperation with absolutly no emulsion. there was some haze in the biodiesel like it looks when I start to wash, it goes sort of milky yellow with lots of tiny little bubbles, this will become crystal clear and even lighter yellow than it began if allowed to settle for a while (usually a day or two). at 40 degrees F 150mL sample separated in 12m 4s, there was gunk in emulsion in the FAME on top that never settled out, after about seven minutes it had separated into 60/40 (the 60 being BD) with lots of emulsion in the biodiesel layer, this emulsion never really broke but it reached about 55/45 by the 12m 4s point at which point it was as complete as it got within the 40m before I disposed of it. I don't think that I would say this passed because of the junk in the top layer and also because it never really came back to 50/50. some questions remain: this test clearly tests for three things: soap, monoglycerides, and diglycerides. how can we test for triglycerides (really incomplete reaction)? if we look at the results and say this didn't pass we should have some path for figuring out why. what methods can be used to tell the difference between excess soap and unreacted mono and di glycerides? do we learn anything from the separation time itself on a passing batch? is 4m fuel better than 10m fuel? ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/ ___ Biofuel mailing list [EMAIL PROTECTED] http://wwia.org/mailman/listinfo.cgi/biofuel Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Biofuel archives at Infoarchive.net (searchable): http://infoarchive.net/sgroup/biofuel/
Re: [Biofuel] more on the quality test
somone on the yahoo groups list (can't find the message right now, I will post a link when I do) posted results of lab tests that showed low mono or di glycerides but a high level of triglycerides. I admittadly don't understand the chemistry well enough to know why that would happen (or even if it could). perhaps really bad stirring such that part of the fluid volume never became involved in the reaction (is that possible?). Incomplete reactions occur for several basic reasons. 1) Insufficient catalyst, 2) Insufficient alcohol, 3) Insufficient duration of reaction, 4) Insufficient agitation and 5) Feedstock exceedingly high in FFAs, all of which are easily overcome. As well, triglycerides don't appreciably emulsify as do mono- and di-glycerides. which is specifically why I am intarested in a test for them. suggestions that I am barking up the wrong tree are welcome :) If you've got triglycerides remaining you'll also have the emulsifying mono- and di-glycerides, primary emulsifiers. If you've got no emulsifiers present, then you're going to be very hard pressed to find any registerable amount of triglycerides. It's really an either/or scenario. This is where a wash test is a fair indicator. If emulsion forms using water of room temp, presuming sufficient settling time has been conducted (and better still if the reaction was a/b), then you know you've got incompletely reacted mono- and di-glycerides. Whether or not you know the molecular ratio of each, much less that of any tri-glycerides is relatively a non-issue. If it's precise measurements you seek, you're not going to find a homebrew test that will give you any answer. I am less concerned with altering the process to achieve less soap (it seems to produce little enough as it is, provided that you use the right amount of lye) than I am with finding a method to tell the difference between an underreacted batch and a soapy batch, Well, if that's the case, I'd have to say that you've got your priorities out of order. Soap is a variable/emulsifier. It's a variable that competes with other emulsifiers. It's also a waste product that has to be dealt with, to the tune of 6% - 25% of original feedstock volume, depending upon how abused the feedstock is. Best to eliminate and/or reduce variables and waste products wherever possible. Do you want to make soap or do you want to make biodiesel? something like soap emulsifies BD into the water and you get a larger amount of water after settling wheras underreacted emulsifies into the BD so you get a larger top layer Emulsification is just that. It reduces visible volumes of both water and fuel, adding itself as the mid-layer. An emulsion may break over time, with or without treatment. But you'll never have a larger volume in either the water or fuel layer. the answer is reprocess a sample of the batch that failed and look for glyc to drop out, if it dosen't you have soap problems, That's not true. Soap drops with the glyc. If nothing drops then you have no problem. if it does you have underreacted your batch. this may also be my test for triglycerides. No. It just tells you that you had an underreacted batch, not the ratios of underreacted components. I understand, but perhaps having a sense of really great fuel will separate within 4 minutes at 70 degrees wheras less good but passable fuels will separate in 10 or more minutes with the outside limit of pasability being 30 minutes would be helpful. You want a green light so that you can run incompleted fuel through your engine? Why not strive for completed reactions rather than outs? If it's outs that you want, you might keep in mind that many people are running SVO, WVO and even animal fats through their diesels. Those are all virtually 100% incomplete reactions, are they not? But then again, a non-reaction is not going to yield the same end product as an incomplete reaction. People running SVO or WVO don't run into problems derived from soap, emulsion, residual catalyst or residual methanol. Which means that a biodieseler really needs to possess an understanding of how to keep their meddling from becoming problems in the first place - which means stop making soap, stop any practice that lends to incomplete reactions and get a cleanly washed product. It's really that simple. Todd Swearingen A biodieseler's biggest concerns are getting all the methanol, soap and catalyst out of the fuel - Original Message - From: John Guttridge [EMAIL PROTECTED] To: [EMAIL PROTECTED] Sent: Wednesday, December 29, 2004 10:21 AM Subject: Re: [Biofuel] more on the quality test Todd, Thanks for the responses. lots of good information, more questions follow. I understand that I sound like a little kid going why to everything you say but I really want to understand what I am doing here so that I can be a shining example of the products of the homebrew community and all it has
