Author Topic: 10/90 dropout test modification for better conversion  (Read 9646 times)

Offline dgs

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10/90 dropout test modification for better conversion
« on: September 29, 2016, 11:38:02 PM »
I should really make notes so that when I post some thoughts about the process the information seems to flow more logically - but I don't! It just comes from the grey cells (or whatever is left of them) So I will try and make
this as simple as possible.

I water wash quite aggressively with a compressor line at the bottom of the wash tank. After a wash which is usually a max of 20 mins per go I drain the water after settling. The dreaded emulsified mono layer is sometimes hardly noticeable and at other times it is considerable.

To create biodiesel the oil (triglyceride) molecule has to have the three fatty acid chains stripped from the glycerine molecule, which happens in sequence. When one acid chain is left, this monoglyceride molecule will be left in the biodiesel unless it is also converted, leaving the glycerine molecule.

If there is any unreacted oil left in the mix there will be a higher proportion of di and monoglycerides left as well.

According to tests done some years ago by gas chromatograph the methanol phase in our 10/90 tests can hold up to 2% oil even though it is clear, so when we conduct a 10/90 test we don't know if the methanol is free of oil or if it contains the 2% (in which case there will be a higher % of di and monoglycerides present)

A batch of bio that was processed some weeks ago washed really well with hardly any mono's showing. The batch I completed a few days ago was an absolute swine to wash with a considerable emulsified layer showing.

I decided to try some higher concentration variations of the 10/90 test on these 2x batches. Firstly the batch that washed well (low mono's) I first did a 20/80 which was clear, then a 30/70, then a 40/60, all the tests were totally clear with an immediate clear methanol phase.

Now to the hard to wash batch (high mono's) I only had to do the 20/80 test which showed 3.2 mls of dropout. Yes 3.2 mls I could hardly believe it. Let me say at this point that both batches showed a clear 10/90

If the poor batch really had the 2% of oil left in the methanol phase of the 10/90 then increasing the bio amount in relation to methanol would have resulted in some oil coming out of solution and because of the high amount of biodiesel dissolved in the methanol some of this would rather mix with the oil than stay in the methanol. Hence the massive dropout.

So, it seems that after a clear 10/90 if we do a 20/80 it will tell us if some oil still remains in the bio and (more importantly) how well we can expect it to wash.

We cannot use the 20/80 test to calculate the catalyst amount for a re-process and if the 20/80 is a fail and the 10/90 was a pass then how much catalyst do we add. Logically I would say 0.5gms/litre if using potassium. 0.3gms/litre for sodium and 1.0mls/litre for ASM.

Before anyone says 'why should we bother with all that extra complication' I do appreciate having really well converted bio can be said to be over doing it if using older vehicles, also for those who don't water wash the above is not as significant. However, for water washers, passing the 20/80 test will certainly make the washing process easier.

Quick after thought, having 2x dropout tubes for the above tests makes things a whole lot easier

« Last Edit: September 29, 2016, 11:43:44 PM by dgs »
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Offline Bill

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Re: 10/90 dropout test modification for better conversion
« Reply #1 on: September 30, 2016, 08:06:27 AM »
If there is space in your measuring deice just add more bio to your 10/90 test to make the 20/80 ratio based on 90 ml of methanol. I think it works out at an extra 12.5ml of bio to add. I do my test in a jar so adding extra after the 10/90 is not a problem.
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Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #2 on: September 30, 2016, 09:28:29 AM »
That is a really good idea Bill, so it is like two tests in one, thanks.
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Offline Jamesrl

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Re: 10/90 dropout test modification for better conversion
« Reply #3 on: September 30, 2016, 02:32:23 PM »
Me and me mate Gord have been doing this trick for years, we try to out do each other with who can get the most bio into a 10/90 before we get a dropout.

IIRC I got to 40/60ish once.

Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #4 on: September 30, 2016, 03:02:17 PM »
As I have now found Jim, bio and methanol are not miscible in all proportions, regardless of how well the bio is converted.

This is not immediatley obvious when the tube is shaken as the two liquids stay miscible for quite a while but if the bio concentration is more than (as you say) something like the 40% region the liquid will split into 2x phases but it takes time, something like 48 hours.
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Offline DavidShinn

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Re: 10/90 dropout test modification for better conversion
« Reply #5 on: September 30, 2016, 05:12:39 PM »
Excellent idea Dave. Well worth doing the 10/90 and 20/80 tests and taking time to get as much conversion as possible prior to washing. My current jelly batch (rescued following your advice) has washed so easily due to it being fully converted. I've had some batches that must have only just passed the 10/90 that have been somewhat of a nightmare to wash.

Will try your test on my next batch.


David

Offline Bio-boy

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Re: 10/90 dropout test modification for better conversion
« Reply #6 on: October 09, 2016, 02:08:09 PM »
I've just tried this exact test so I will report back my findings.  ;)

Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #7 on: October 09, 2016, 04:15:58 PM »
I've just tried this exact test so I will report back my findings.  ;)

BB, with double the amount of bio in the mix the test is very temperature sensitive, make sure you do it at 20 degs if you can.
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Offline Bio-boy

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Re: 10/90 dropout test modification for better conversion
« Reply #8 on: October 09, 2016, 04:31:33 PM »
Absolutely no fall out 2 1/2 hours later albeit the temp taken with my laser is 14.2deg.
Not too sure what the effect of temp +-20 deg will make.
However, I'm sure one of the more experienced amongst us will inform me.

Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #9 on: October 09, 2016, 05:12:31 PM »
The test is harder to pass the colder it gets (10/90) but doing a 20/80 at lower temps could mean any dropout you were seeing would be mostly bio with some methanol, whereas the top phase would be mostly methanol with some bio.

Leave it all night to get colder, but if it has been 2 1/2 hours it is looking good. you have proved it is a very good pass, probably >99% conversion. Min ASTM 14214 is 96.5% min.
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Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #10 on: October 11, 2016, 10:32:52 AM »
This is my reply to Element from a thread presently on VOD ;Water washing discovery.

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Hi Element,

I totally understand what you are saying. When I have used acid in the recent past I have done a similar thing, reducing the acid per wash.

If most of the emulsified layer has been removed then the mono's will be greatly reduced, but not removed completely.

Even if a hard wash reveals no mono's there will still be some present. The nature of the reaction is such that they can't be totally avoided.

The EN spec for mono's is 7000ppm (0.7%) the other specs for di's and tri's are tighter than this. As the mono's are the last stage before the bio (FAME) they are the most difficult intermediate to totally get to react.

A friend ex the infopop forum who has become a biopowered member posted a thread which had several graphs of the reaction, (mathmatical models) showing the unreacted intermediates.

From his models if a 10/90 is clear but 'on the cusp' and the methanol phase is holding the 2% of tri's (which is possible even with a clear test) then the mono's are about 2.2% (22000ppm) Three times more than the max spec.

I think the important point to mention here is that having mono's this high would make the bio 'over spec' on bonded glycerine, which is why it is important to remove them.

So as you can see there is no wonder we get the considerable emulsified layer when doing a 'hard' wash, even after a totally clear 10/90

Increasing the bio ratio in the 10/90 seems to work but makes the test very temperature sensitive. A clear 20/80 usually gives a better wash with hardly any mono's showing (but not always) I will keep working on it.
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Offline Bio-boy

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Re: 10/90 dropout test modification for better conversion
« Reply #11 on: October 11, 2016, 08:32:43 PM »
Checked 20/80 test again today and still no fallout!  ;)

Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #12 on: October 11, 2016, 10:34:14 PM »
Checked 20/80 test again today and still no fallout!  ;)

Great news. My last attempt didn't work too well, maybe my batch just wasn't converted enough. Your result has given me new hope.
« Last Edit: October 11, 2016, 10:36:50 PM by dgs »
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Offline dgs

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Re: 10/90 dropout test modification for better conversion
« Reply #13 on: October 12, 2016, 06:52:08 PM »
I am presently processing a small experimental batch to test the 20/80 test further. The testing will also include a different 10/90.

To Explain, today I added 12 mls of new rapeseed oil and 240mls of virgin methanol into a 250ml separating tube. I gave it a really good shake for a few mins and left it to settle. Tomorrow I will run off the oil and the methanol will be used for one of the 10/90 tests.

The idea is that as the methanol is (presumably) now saturated with oil, using it for the 10/90 test should give a more accurate drop out.

I will do 3x dropout tests on the batch tomorrow after S2 (I have 3x dropout tubes)

One will be a 'normal' 10/90, One will be a 10/90 with the tri saturated methanol and the third one a 20/80

i will report when the tests are completed.
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Offline Julian

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Re: 10/90 dropout test modification for better conversion
« Reply #14 on: October 12, 2016, 07:53:42 PM »
Sounds interesting, Dave.  Looking forward to the results.

We did have Jan Warnqvist sign up on here a little while back so I guess you could contact him via pm (which I assume will result in an email notification) if advise is needed.
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