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  #1  
Old 02-06-2009, 06:09 PM
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1st batch fails 27/3 test.

After having it sit in the reactor for over a week, I fiinally got around to testing it. It did get below freezing for a few days, and is now in the 50's, if that makes a difference. In the sight tube it looked good, I could actually read through it. However there was about a half inch of clear fluid on the top. According to a previous post, Fabman said this was probably soap. I shook it in the tube, and it did become like soapy water, so I'm assuming that it is soap. The 27/3 test was done, and as the pic's show, it became cloudy after shaking for 5 sec. After sitting in the flask for about 10 minutes, there is a blob of oil on the bottom, and the solution is less cloudy, so some of the 3 ml has fallen out of solution. Hope these pics attach.
Anyhow, how did I manage to get underreaction and soap at the same time?
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  #2  
Old 02-06-2009, 06:37 PM
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This is wierd, the "blob" just fell apart and went back into solution? On another forum, it was suggested that I might have a "false fail" due to not having heat the oil up to room temp. Anyway the solution is probably is getting close to room temp now.
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Old 02-06-2009, 08:30 PM
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It is possible to make soap, and still have an incomplete reaction. Did you do a "sizzle" test on your oil? Water is the most likely suspect. Just because you can't see any water in the oil doesn't mean there's NO water present. It only takes .05% H2O to cause problems.

What tends to happen with excess water present is the water "pulls" some of the lye out of the methoxide solution to form soap, leaving less catalyst for the reaction.

You should be able to save this batch by reprocessing using a couple of gallons of Methanol and 3-5 grams/liter of lye.

Are you using KOH, or NaOH, and have you removed the glycerol already?
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Old 02-06-2009, 09:42 PM
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We used KOH, and the Glycerine has been saved in another container. We used the 80/20 method, if that makes a difference. Was thinking of re-heating the bio while running the reactor to drive off any water.
It's been a couple hours now, and after reshaking the mixture in the flask the oil seems to be remaining in suspension.
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Old 02-07-2009, 09:51 AM
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It sure looks too cloudy ( read "unreacted") to me..............

It should look like this:

Click the image to open in full size.
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Old 02-07-2009, 10:46 AM
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Think I'll try the test again. "When in doubt, read the instructions". After sitting overnight, I shook it up again, and this time it stayed in suspension. The 27/3 solution isn't exactly clear, but if I set the flask over a piece of paper, I can read through it. Still will have to deal with the soap issue...
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Old 02-07-2009, 11:06 AM
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Also will take a sample and do the sizzle test as you recommended, we thought that we had all of the water out of it. We have a settling tank setup before the reactor with the outlet about 15 gallons up from the bottom, so the good oil goes into the reactor and the water and junk goes to the bottom. We ran the reactor about three hours @ 145 (hottest we could get it) until there wasn't much distillate coming out of the condenser...
Will add more insulation to see if I can get up to 155, but that's as high as the thermostat goes.
Will have to post some pics sometime.
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Old 02-07-2009, 11:12 AM
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I don't use a waterheater thermostat in my system. I found that the waterheater thermostats use a "snap" switch, and can drop as much as 20 deg before comming back on. I use a oven thermostat which only drops about 2-3 deg before comming back on. Much better temp control, and I can turn it up over 210 deg to boil all the water out first.
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Old 02-07-2009, 11:16 AM
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Hmm, I like that idea. With a partial vacuum and 3500 ft elevation, that should easily be hot enough to boil off water. Will pass that on to my partner... thanks again!
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Old 02-07-2009, 11:17 AM
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Quote:
Originally Posted by Trent Fliginger View Post
We ran the reactor about three hours @ 145 (hottest we could get it) until there wasn't much distillate coming out of the condenser...
If you where getting distillate from your condenser, you most certantly had water in the system.

145-155 deg is not enough to remove the suspended water...........
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Old 02-07-2009, 11:20 AM
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Quote:
Originally Posted by Trent Fliginger View Post
Hmm, I like that idea. With a partial vacuum and 3500 ft elevation, that should easily be hot enough to biol off water. Will pass that on to my partner... thanks again!
At your elevation, 20" of vacuum would pull all of the water out
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Old 02-07-2009, 11:20 AM
 
 
 
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