Passed PHLIP and Methanol Test FIALED in the Lab for gly. (pictues)

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can't get pictures to load it says only 50kb allowed

Registered: 13 April 2009

Ignored post by 2000psdbio posted

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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: 13 April 2009

Ignored post by 2000psdbio posted

RickDaTech

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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.

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Ignored post by RickDaTech posted

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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: 13 April 2009

Ignored post by 2000psdbio posted

Andrew M

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quote:
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

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03 Dodge 2500 B100 homebrew
79 Rabbit B100 homebrew

Location: Northern California | Registered: 27 February 2006

Ignored post by Andrew M posted

Green energy

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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: 17 February 2009

Ignored post by Green energy posted

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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: 13 April 2009

Ignored post by 2000psdbio posted

Green energy

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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: 17 February 2009

Ignored post by Green energy posted

Green energy

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Posted

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: 17 February 2009

Ignored post by Green energy posted

Andrew M

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Posted

quote:
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: 27 February 2006

Ignored post by Andrew M posted

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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: 13 April 2009

Ignored post by 2000psdbio posted