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Passed PHLIP and Methanol Test FIALED in the Lab for gly. (pictues)
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Well here it is the pictures are 40 minutes after each test was done. Mirror finish and bio nor indicator is even slightly foggy. The methanol test was done with 225/25 and after 40 minutes there is not even a small drop. The feedstock was about 25% virgin canola and 75% lightly used vegetable oil titration was 1.2. I used a base/base and it was very close to passing methanol test the first time. We processed it at 170 degrees and about 25psi pressure with mixer and pump for 45 minutes each time, so im not sure how we did not get a complete reaction. Then I mixed 5% water back into the first glycerin and added it back into the bio to kill the reaction. Waited and drained off the gly/water. Then I pulled 25’’ hg vacuum at 180 F for about an hour to pull out the water /methanol. Sandy brae showed about 80ppm water. Then the bio was ran through woodchips-thermax-purolite-coldclear. It gets filtered about 4 times between all this. I am Appling to be a biodiesel producer with the epa/irs and the IRS came to my facility to get a sample of fuel and they just notified me of the results:

-1.6% total glycerin (they don’t know the breakdown)
-Whatever else they tested was fine.

I had my own sample done back in may for the national biodiesel board. I paid for the full astm d6751-08 and passed all tests the first time. Total glycerin was only at .16%. The PHLIP test and methanol test looked the same then as now, but they tell me I have 10X more glycerin. I am willing to take the blame if something was wrong but all this makes me wonder if someone else made a mistake. Im not even sure how to change my process to make the test pass.



 
Registered: April 13, 2009Reply With QuoteReport This Post
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can't get pictures to load it says only 50kb allowed
 
Registered: April 13, 2009Reply With QuoteReport This Post
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The irs mailed the results and i guess there was 1.6% mono di and triglycerides(no breakdown) left over and the total glycerin was .315 which is still more than I expected since it passed both methanol and phlip tests so well.
 
Registered: April 13, 2009Reply With QuoteReport This Post
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If you send off a sample to 10 different labs, you will get 10 different results for total glycerin. However I doubt that there will be anything close to a 10X difference. I would challenge the IRS results and ask them to repeat the test.
 
Location: Cowboy Country | Registered: December 06, 2004Reply With QuoteReport This Post
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The samples that i sent in were different sample but as i said both passed phlip tests and methanol tests and i guess the irs guys was a little confused on the phone he told me i had 1.6% glycerin, but he ment 1.6% oil which equated to .31% gly. which is still to high but at least its in the ballpark. I guess next time i'll hit hit with a third stage with a small amount of methoxide. Or maybe try acid/base/base
 
Registered: April 13, 2009Reply With QuoteReport This Post
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The methanol test was done with 225/25 and after 40 minutes there is not even a small drop.


Very interesting results.

Do you control the temp., and if so how and to what temp.?


Andrew

http://biodieselcommunity.org
03 Dodge 2500 B100 homebrew
79 Rabbit B100 homebrew
 
Location: Northern California | Registered: February 27, 2006Reply With QuoteReport This Post



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I would guess the temperature is too high. Better not higher than 150 F.
Why you like high temperature? High temperature may increase the speed of esterification, but also, it helps make soap. Under higher temperature, the ester is very easy to react with the sodium hydroxide to make soap. Also the esterification goes back under high temperature.

You need to balance the temperature. Too low need longer time, too high makes more soap and total glyncerides.

(I remember I read some data of the ISU group, it shows the lower temperature get lower total glycerides number.)


quote:
Originally posted by 2000psdbio:
Well here it is the pictures are 40 minutes after each test was done. Mirror finish and bio nor indicator is even slightly foggy. The methanol test was done with 225/25 and after 40 minutes there is not even a small drop. The feedstock was about 25% virgin canola and 75% lightly used vegetable oil titration was 1.2. I used a base/base and it was very close to passing methanol test the first time. We processed it at 170 degrees and about 25psi pressure with mixer and pump for 45 minutes each time, so im not sure how we did not get a complete reaction. Then I mixed 5% water back into the first glycerin and added it back into the bio to kill the reaction. Waited and drained off the gly/water. Then I pulled 25’’ hg vacuum at 180 F for about an hour to pull out the water /methanol. Sandy brae showed about 80ppm water. Then the bio was ran through woodchips-thermax-purolite-coldclear. It gets filtered about 4 times between all this. I am Appling to be a biodiesel producer with the epa/irs and the IRS came to my facility to get a sample of fuel and they just notified me of the results:

-1.6% total glycerin (they don’t know the breakdown)
-Whatever else they tested was fine.

I had my own sample done back in may for the national biodiesel board. I paid for the full astm d6751-08 and passed all tests the first time. Total glycerin was only at .16%. The PHLIP test and methanol test looked the same then as now, but they tell me I have 10X more glycerin. I am willing to take the blame if something was wrong but all this makes me wonder if someone else made a mistake. Im not even sure how to change my process to make the test pass.



 
Registered: February 17, 2009Reply With QuoteReport This Post
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Interesting stuff there greeen energy i have never heard of anyone having too high temp so i just process at a prety high temp under pressure it seems to speed the reaction a lot, i used to do a base/base and mix for 30 min each time and it passed methanol test easy. Wont processing for too long allow back reactions? I may try some batches at 150 and see if the results are different.

My methanol test is done with the biodiesel still warm probably 130 and the methanol about 65-68.

O yeah after letting the methanol test set for 24 hours there are some small things that float-not on top but in the biodsiesel/methanol. They wont sink either. So im not sure what it is i think it is just from the hydronated freedstock.
 
Registered: April 13, 2009Reply With QuoteReport This Post
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Yes, just try a lower temperature. I belive the yield will be higher, the total glycerides will be lower.

A longer time should be not a problem, at least I never heard of that. Too high temperature is not a good idea for the base reaction. (Normally, increase 10 degree double the reaction speed, but the esterification goes back when T>70 celsium...)

3-27 test normally is done at room temperature, higher temperature just make the tri-glyceride more solutable.

quote:
Originally posted by 2000psdbio:
Interesting stuff there greeen energy i have never heard of anyone having too high temp so i just process at a prety high temp under pressure it seems to speed the reaction a lot, i used to do a base/base and mix for 30 min each time and it passed methanol test easy. Wont processing for too long allow back reactions? I may try some batches at 150 and see if the results are different.

My methanol test is done with the biodiesel still warm probably 130 and the methanol about 65-68.

O yeah after letting the methanol test set for 24 hours there are some small things that float-not on top but in the biodsiesel/methanol. They wont sink either. So im not sure what it is i think it is just from the hydronated freedstock.
 
Registered: February 17, 2009Reply With QuoteReport This Post
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You mentioned that at first time, you passed the total glycerol test, what is the process temperature at that time?

Thanks.

quote:
Originally posted by 2000psdbio:
Interesting stuff there greeen energy i have never heard of anyone having too high temp so i just process at a prety high temp under pressure it seems to speed the reaction a lot, i used to do a base/base and mix for 30 min each time and it passed methanol test easy. Wont processing for too long allow back reactions? I may try some batches at 150 and see if the results are different.

My methanol test is done with the biodiesel still warm probably 130 and the methanol about 65-68.

O yeah after letting the methanol test set for 24 hours there are some small things that float-not on top but in the biodsiesel/methanol. They wont sink either. So im not sure what it is i think it is just from the hydronated freedstock.
 
Registered: February 17, 2009Reply With QuoteReport This Post
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My methanol test is done with the biodiesel still warm probably 130 and the methanol about 65-68.


I suggest doing the 3/27 again, on washed and dried fuel with all of the elements of the test maintained at 66-68f. Please let us know what you see. The temp of the test is, IMO, critical.


Andrew

http://biodieselcommunity.org
03 Dodge 2500 B100 homebrew
79 Rabbit B100 homebrew
 
Location: Northern California | Registered: February 27, 2006Reply With QuoteReport This Post
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Ok, i have redone the methanol test at 66 degrees and for bio and methanol, it passed IMO. After 20-30 minutes there is some very fine "dust" on the bottom When i heat the sample it goes away, so im not sure if it is esters or unconverted glycerides.
The other sample i had tested was procesed at 150 degrees at atmospere pressure and i used a different processor that has a little better agitation. It was also base/base.
 
Registered: April 13, 2009Reply With QuoteReport This Post



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Did they use a GC or did they use some other method (impedence spectroscopy, infrared)? The newer technologies such as IR and IS may not tell you the breakdown, but if your lab did GC they ought to be able to tell you what the free glycerol, mono, di, and tri glyceride breakdown.

It is not unusual to pass both the phlip test and the 3/27 test, then fail the ASTM analysis. While triglycerides are not soluble in methanol, mono and diglycerides are to a large extent soluble in methanol. Free glycerol is pretty much completely soluble in methanol. Even in well-reacted fuel, mg and dg are almost always higher than tg, and you could have theoretically 1% or more mg/dg and not be able to tell the difference in the 3/27 test or the phlip test.

MGs/DGs will not show up in the 3/27 test to any measurable degree, and those are usually the highest constituents. If you have "turbidity" you may have a significant quantity in there. Free glycerol may turn the methanol slightly brown, but the resolution window of 0.02% may not be detectable to the human eye. The Phlip test will give you some indication of glycerides in the fuel but again not to any measurable degree.

As to the 3/27 test, have you tried increasing the scale to, say a 9/81 test? B/c if you see even 0.05 mL/9mL is 0.56% triglycerides, which likely means you will probably have even higher diglycerides and higher still monos. If you don't have that kind of measurement, increase it even higher to say 90/810 (then if you can see 0.1 mL, it's still somewhat high).

Sadly, it is typical to submit to multiple laboratories and get multiple results, no matter how consistent your sampling is. Sample points (where and how you sample) as well as sample preparation is the most common culprit, and the fact that some peaks can be misidentified if the lab is using a software package to identify the peaks automatically. It's also therefore not unusual also to get bad results, as a previous poster mentioned. But if I were to submit a sample of fuel to an outside laboratory for free and total glycerin analysis, had consistently 0.2% total or less, and they told me it was as high as 1.0% but they couldn't even tell me the breakdown, I would ask for a certificate that shows which laboratory they used and whether the IRS followed the ASTM method. When you get a cert of analysis elsewhere, they usually put down the mg, dg, tg and free glycerol.

This is good information for us producers who are pursuing the tax credit, I am a little concerned about whether the IRS is actually doing the test properly and getting good results since as I understand the tax credit is relatively new.

This message has been edited. Last edited by: emily e,
 
Registered: October 13, 2006Reply With QuoteReport This Post
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Then I mixed 5% water back into the first glycerin and added it back into the bio to kill the reaction. Waited and drained off the gly/water. Then I pulled 25’’ hg vacuum at 180 F for about an hour to pull out the water /methanol. Sandy brae showed about 80ppm water.



so why add the 'first' glycerin back in??

your not water washing???

sound to me like you had a reverse reaction..

processing temp..I disagree with others here..the hotter the better as long as you don't loose methanol..if you loose methanol during the process all bets are off!! FYI I have processed at 170F at 0 PSI without a problem..

to fail at those numbers is shocking. since you passed 27/3

but like Andrew as asking at what temps??

-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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Originally posted by emily e:
I am a little concerned about whether the IRS is actually doing the test properly and getting good results since as I understand the tax credit is relatively new.



The tax code states that in order to be eligible for the refunadable tax credit you must: (1) be registered with the EPA, and; (2) produce ASTM specification fuel.

My advice is to anybody trying to get licensed is to have your tax attorney send in a copy of your independent ASTM lab report (the same one you send to the EPA with your NBB info) and EPA registration with your application and be prepared for a drawn-out fight.
 
Registered: April 08, 2009Reply With QuoteReport This Post
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I processed the batch at higher temps i want to say it was 160. The reason i added the glycerin back in was to prevent an emulsion when i did a 5% prewash. I do a prewash because I am afraid of back reactions. Which is why i am not sure how i could have gotten back reactions with a 5% prewash. As for the lab it was a national lab in Washington state-run by the government...that’s always good.
I have since sent in another sample that looks the same in the 3/27 test which is actually a 450/50 test when i do it. No traces of anything falling out of the 50ml for at least two hours...the same as the first sample i did. When i do this i am super picky-i wash the jar out threee times with clean methanol to make sure there is not leftover residues, an if i see the smallest amount of anything(dirt or contaminates that are not oil) in the sample i dump it and re-due the sample to make sure i have got complete reaction. This sample came back as .165 total gly compared to .31 for the first sample. It also again passed the phlip test and it came back with a acid number of .57 and oxidative stability of .1 yes .1 not 1 hour. This caught me way off guard because i have never had any trouble with either of these tests.
I sent the folks at cytoculture a sample of fuel and two of my phlip tests, and they have been working on it for about three weeks and last i talked to them was on the 21st of dec and they still are trying to figure out what is going on.



My advice is to anybody trying to get licensed is to have your tax attorney send in a copy of your independent ASTM lab report (the same one you send to the EPA with your NBB info) and EPA registration with your application and be prepared for a drawn-out fight.

I ask them this question and they don’t care about your independent lab results they will do their own testing(at a government lab) and they have to visually see you pull the sample out of a storage tank. Now i am asking myself why did i bother since they have not even extended the tax credit.
 
Registered: April 13, 2009Reply With QuoteReport This Post
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I have since sent in another sample that looks the same in the 3/27 test which is actually a 450/50 test when i do it. No traces of anything falling out of the 50ml for at least two hours...


Questions:
Do you control the temp. of the 3/27 test?
If so, how?
At what temp.?

Can we see the a pic of the test results?
Or did you get the #'s verbally?


Andrew

http://biodieselcommunity.org
03 Dodge 2500 B100 homebrew
79 Rabbit B100 homebrew
 
Location: Northern California | Registered: February 27, 2006Reply With QuoteReport This Post
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the IRS is a bunch of thugs, I would put nothing past them. They probably made an error and won't admit it.



 
Registered: April 28, 2008Reply With QuoteReport This Post



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i would love to post some pics of the phlip test and the test results, but im not sure how to post pics on here.
 
Registered: April 13, 2009Reply With QuoteReport This Post
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If you want to make things easier just do a titration for left over caustic after your reaction, then use acid to neutralize it, no caustic, no reverse reaction.
 
Location: West Michigan | Registered: April 26, 2006Reply With QuoteReport This Post
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