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3/27 Experiment
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Hello Folks
Hoping to get some input from those of you that do the 3/27 test regularly. I normally set up a 50/200 test beside me to watch while I perform my SAFTEST reading just as a double check (I don't trust SAFTEST).

I did the following on a 90% reaction. (Think 80/20 but I did a 90/10)
50/200 test=56% unconverted

I then heated the oil to about 110C for about an hour and did the test again
50/200 test=26% unconverted.

That's too big a difference to be due to methanol removal alone, and it also only occurs when I have an AE. Not really an issue just something I have noticed. Anyone have an explanation for this? Water from the AE?
 
Registered: February 25, 2010Reply With QuoteReport This Post
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Brad
could it be that as the temp increased the reaction kicked into high gear? did you do anything to this batch to stop the reaction, like 5% pre wash, prior to demeth? Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Doubtful since I didn't get much glycerin drop out. I'd have expected a good layer in the bottom of my beaker from that much of a change. This was just done on a 500mL sample I had taken off too so no prewash or anything on it. Just took the sample did the 50/200, heated while doing other things then came back and did the 50/200 again. Both tests at 23C as well.

This message has been edited. Last edited by: BWilder,
 
Registered: February 25, 2010Reply With QuoteReport This Post
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Brad
-I'm at a loss, conversion has increased as indicated by your version of 3/27, to a point where you now have 26% unconverted oil, which means the process has moved further to the right the only differance in the two samples is the second sample had more heat and longer process time? It is not uncommon in my experiance to have little or no dropout in the second reaction, the byproduct stays in suspension.
-with the methanol boiled out of the first oil sample the % of biodiesel/wvo would by higher in relation to the methanol added for the test, and therefore one would expect an even higher dropout amount than the 56% indicated in the first test.
-either the first test result was incorrect or more conversion has taken place
-50/200 = 1 part bio to 4 parts methanol: 3/27 = 1 part bio to 9 parts methanol. given the variation in bio/methanol concentration how do you determine the % unconverted or did I miss something here Confused Tom


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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hmmm no edit function for previous post!
Brad
-do we know for sure that methanol has the ability to disolve 25% biodiesel by volume and keep it in suspension?


" I don't know what I don't know until I know"
1994 GMC 6.5 Tubo 2005 Dodge ram 3500, 3 VW's 2000, 2002, 2005.
 
Location: Manitoba Canada | Registered: March 24, 2009Reply With QuoteReport This Post
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Hi Tom
I'm positive I can get a pass on 50/200 as I have seen several crystal clear samples previously. After my second reaction I normally get a crystal clear or sometimes slightly hazy sample. That said I'm a newbie at this test. So still learning. I normally relied on SAFTEST readings. Just trying to add another check to my system since I really don't like that there is no feedback on the SAFTEST for a failed sample.

I tried it again today with the next batch.
Initial reading 50/200=42%
After heating/cooling 50/200=18%

I do this in a 250mL graduated cylinder so every tick on the glass is 4% which is why I am comfortable with 2% increments. I also tried the second test using a 500mL cylinder. So a 50/450 test, the graduations on the bigger cylinder don't go low enough but it looked like 18% just 'eyeballing' it.

For info diesel was 1/3 yellow grease 1/3 beef tallow 1/3 chicken fat.

edit: I actually had a test show unreacted when it was fully reacted previous to me attempting this (its what prompted the experiment) I thought a batch was under reacted added more methoxide and just made more soap no glycerin.
 
Registered: February 25, 2010Reply With QuoteReport This Post



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you do know that the 27/3 was started as 225/25..a 9/1 ration..at 225/25 a 1ml fall out indicates a 99% conversion. I'm just wondering where you got the 50/200 numbers?

so when you heating to 110c are you just trying to remove methanol? to get all the methanol out you need more like 127C or more...during the heating you'll drive the reaction more to completion, before the critical amount of methanol is gone. this might be what you're seeing.

-dkenny


'84 bluebird school bus, DD8.2L turbo( 4/2011, the bus tranny has died..Frown 8.23.11 bus driven to scrap yard Frown )
2006 Jeep Liberty CRD Smile - the wife's
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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quote:
Originally posted by dkenny:
you do know that the 27/3 was started as 225/25..a 9/1 ration..at 225/25 a 1ml fall out indicates a 99% conversion. I'm just wondering where you got the 50/200 numbers?

so when you heating to 110c are you just trying to remove methanol? to get all the methanol out you need more like 127C or more...during the heating you'll drive the reaction more to completion, before the critical amount of methanol is gone. this might be what you're seeing.

-dkenny


Hello DK
That I was actually unfamiliar with. My numbers are based on dropout which I was assuming was directly correlated to % conversion. So 18% unconverted corresponded to 9mL of dropout. 56% unconverted was 26mL dropout.

I still don't think it was driving the reaction to completion however, the sample had no catalyst in it which I am assuming is required and I had no visible glycerin dropout after heating and cooling.
 
Registered: February 25, 2010Reply With QuoteReport This Post
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quote:
Originally posted by dkenny:
you do know that the 27/3 was started as 225/25..a 9/1 ration..at 225/25 a 1ml fall out indicates a 99% conversion. I'm just wondering where you got the 50/200 numbers?

so when you heating to 110c are you just trying to remove methanol? to get all the methanol out you need more like 127C or more...during the heating you'll drive the reaction more to completion, before the critical amount of methanol is gone. this might be what you're seeing.

-dkenny

dkenny

where did you get the 1ml dropout = 99% conversion from.
The original Jan Warnquist test was indeed 25ml of biodiesel in 225 ml of methanol but he suggested that every 1ml of drop out was equal to 4% unconverted.

Having said that I think a lot of people have questioned the accuracy of this in that the drop out does not give any indication of the mono and diglycerides as they are somewhat more soluble in methanol. THe drop out is mostly triglycerides that are not soluble in the methanol.

Therefore if you have 1ml of fall out in a 25/225 test you are likely to be significantly below the 96% conversion and certainly no where near 99%

This test is a qualitative indication test only not quantitative
 
Location: East Yorkshire | Registered: January 14, 2006Reply With QuoteReport This Post
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fazznag, thanks.brain fart..but i knew the 50/200 was not the right numbers either.
and yes I know the about the mono and di in the test. thanks again

-dkenny


'84 bluebird school bus, DD8.2L turbo( 4/2011, the bus tranny has died..Frown 8.23.11 bus driven to scrap yard Frown )
2006 Jeep Liberty CRD Smile - the wife's
99 dodge 2500 5.9l 24v..-mine Smile
everything run B100 when its warm enough Smile
 
Location: RTP, North Carolina | Registered: December 15, 2004Reply With QuoteReport This Post
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Hello DKenny. I have a question?
When carried out via Esterificacon acid with H2SO4, after completion of chemical reaction, after allowing to stand and measured again with KOH to determine the new H2SO4 acidity does not influence this valuation giving her the wrong amount?

Greetings Jorge Zegarra
Lima Peruy
 
Location: Lima peru | Registered: March 31, 2006Reply With QuoteReport This Post
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