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quote:
Considering we all know warnqvest test is not a reliable means of measuring conversion, what method did you ise to arrive at a conversion of @20%


Just for clarity is that a different test to the Warnqvist test?


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2006 Mercedes C200 CDI (no DPF) B50 (for now)
 
Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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Hi Drum,

quote:
Originally posted by Drum:
Just for clarity is that a different test to the Warnqvist test?
Good to see you are reading my posts.
Spelling mistake corrected. That is the second time I have misspelled his name in the last week.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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quote:
Originally posted by Tilly:
Hi Drum,

quote:
Originally posted by Drum:
Just for clarity is that a different test to the Warnqvist test?
Good to see you are reading my posts.
Spelling mistake corrected. That is the second time I have misspelled his name in the last week.


Well Tilly, as there is never a dull moment when you are around, I always read your posts! And that last one is still inaccurate!


2001 Saab 93 TiD B50
2006 Mercedes C200 CDI (no DPF) B50 (for now)
 
Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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Thank you for your vote of confidence in my knowledge in making biodiesel.One concern I have is that some people continually make inaccurate statements.For instance, It is "common knowledge" that the warnqvest test and all of it's variations is not a reliable measure for conversion. Yet some people who know this continually quote conversion percent based on the warnqvest test.Why do these people knowingly post inaccurate information? It seems these posts are based on the theory that "if you say something enough times, it eventually becomes true" Another concern I have had lately is the recent spate of claims of achieving conversion using remarkably limited amounts of methanol.I know the research done in the past and when someone posts "unbelievably" low amounts of total methanol usage my first reaction is to question how the results were obtained. As it turns out, after doing enough questioning, most of the recent claims of amazingly minimal methanol usage did not actually include All the methanol present in the reaction in the final methanol usage claim.


Your welcome, I mean what I said with all sincerity! My back is another issue, I am learning to cope and each year I seem to be able to do a bit more. I hope to get back into the biodiesel game this year!
the terminology used "conversion" is for sure a misnomer and is the term that has many people questioning the 3/27 test results. Not sure what a better term would be. What is happening now is IMO rather childish, bicker bicker bicker. As adults sometimes we just have to agree to disagree.
I think it would be very constructive if we could define the amount of dropout because a measure of this can be reliably used in calculating the chemicals required in the next process.
I agree the chemicals that remain in the byproduct (how much? who knows?) has not been calculated in the many tests that have been performed. Chemistry say's it takes X amount of caustic and x amount of methanol to achieve the reaction, varying these amounts WILL affect the reaction. On the other hand simply stating that the residual chemical contained in the byproduct reduces the amount of NEW chemical required to complete the reaction would be IMO a true statement.


" 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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Tilly part of the difficulty I have had with you is your infuriating insistance that everything that can be known about making biodiesel is known and has been known for years! Wrong! Simply wrong! And whilst I accept you are very knowledgable and capable of being highly analytical, this single trait has me thinking of you as a retired boxer deciding to make a comeback fight only to find the sport has moved on and it is not the case that 'how it was done in my day'is still the best way to do it. You are more guilty than anyone of saying the same thing over and over again in the hope that it will become truth. This obsession you have with discrediting the Warnqvist test as a means to determine conversion is where I rest my case. 'We do not all KNOW it is unreliable', you keep telling us it is but I can assure you, you don't KNOW! Prove me wrong or stop going on about it. And if you wish to discuss it why not just focus on the thread you started yourself on the matter and then went AWOL when asked to stick to science in your response. I am researching the connection between dropout in the Warnqvist test and how it may be used to give us information on the glyceride distribution (and hence the degree of conversion) of the biodiesel from which the test sample came. And I can assure you the link exists. Whether we can actually get data that can be useful to the home brewer is another matter but I assure you the link exists. As I said before it is not a perfect correlation but the correlation can be determined IF the relative solubility of tri-, di- and mono-glycerides in methanol at room temperature can be determined. If you or anyone else wants to discuss this further I will be only be too happy to indulge you on that other thread.


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Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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Hi Drum,
Your post would be a lot easier to read if you used paragraphs and breaks.

quote:
Originally posted by Drum:
This obsession you have with discrediting the Warnqvist test as a means to determine conversion is where I rest my case. 'We do not all KNOW it is unreliable', you keep telling us it is but I can assure you, you don't KNOW! Prove me wrong or stop going on about it. And if you wish to discuss it why not just focus on the thread you started yourself on the matter and then went AWOL when asked to stick to science in your response. I am researching the connection between dropout in the Warnqvist test and how it may be used to give us information on the glyceride distribution (and hence the degree of conversion) of the biodiesel from which the test sample came. And I can assure you the link exists. Whether we can actually get data that can be useful to the home brewer is another matter but I assure you the link exists. As I said before it is not a perfect correlation but the correlation can be determined IF the relative solubility of tri-, di- and mono-glycerides in methanol at room temperature can be determined. If you or anyone else wants to discuss this further I will be only be too happy to indulge you on that other thread.
From what I can understand from your post, your position seems to be that you think that the Warnqvist test can be used to accurately measure conversion percent, just that no one has been able to come up with a procedure that does it yet and you are currently working on finding that procedure.

When/if you do find this procedure that uses the Warnqvist test to accurately measure conversion percent I can assure you that biodieselers around the world will sing in praise of this accomplishment for many many years and the name "Drum" will be held in an exulted position nearly as great as "Warnqvist" And everyone will bow towards Stroke County in reverence.

But for now I think we need to stick with the idea that the Warnqvist test is not a reliable method of accurately measuring conversion percent.






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post



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If you recover methanol, it does not really make much difference how much methanol you use in the reaction. You will get the excess methanol used back during the recovery.

Yep, thats where I am at, I dont even bother measuring the last 100 litres of recovered methanol I add to my batches anymore, I just eyeball half the drum and any extra gets recovered.
quote:
I think it would be very constructive if we could define the amount of dropout because a measure of this can be reliably used in calculating the chemicals required in the next process.

Herein lies the problem I believe. The feed stock likely has a substantial effect on what is actually dropping out, I doubt an accurate calculation could be made that could be applied to the wide range of WVO out there...
I still cant understand why anyone would want to avoid titrating when it is so simple, so what do I know anyways... Wink
Thats my 2 cents.

Cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Jon, you know a lot, anyone that reads your posts can see that.

I have a 400 litre s/steel proc that I have never used.

A few years ago I was going to set it up and do WBD, but never got round to it.

Am I correct in assuming that when using a sealed vessel for the reaction, advantage can be taken to increase the pressure (and therefore temperature) so the reaction is completed in say as little as @ 10 mins, then just carry on with WBD.
 
Location: YORK UK | Registered: April 27, 2014Reply With QuoteReport This Post
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quote:
Originally posted by Tilly:
From what I can understand from your post, your position seems to be that you think that the Warnqvist test can be used to accurately measure conversion percent, just that no one has been able to come up with a procedure that does it yet and you are currently working on finding that procedure.


In principle definitely, in practice maybe we'll see!

quote:
When/if you do find this procedure that uses the Warnqvist test to accurately measure conversion percent I can assure you that biodieselers around the world will sing in praise of this accomplishment for many many years and the name "Drum" will be held in an exulted position nearly as great as "Warnqvist" And everyone will bow towards Stroke County in reverence.


Now there's an incentive! Are you including yourself? ;-)

quote:
But for now I think we need to stick with the idea that the Warnqvist test is not a reliable method of accurately measuring conversion percent.


I 'almost' agree with this because it is being used fairly reliably to determine second stage chemical usage but perhaps just not precisely because in its current form the test overestimates the amount of chemical required, so assures conversion.


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Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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quote:
Originally posted by Drum:
quote:
Originally posted by Jon Heron:

Herein lies the problem I believe. The feed stock likely has a substantial effect on what is actually dropping out,


Spot on!

quote:

I doubt an accurate calculation could be made that could be applied to the wide range of WVO out there...


Again spot on!

In principle a lab investigation could be done for any pure oil in determining the methanol solubility of its glyceride/fatty acid components at room temperature. Clearly not practical to do that for the range of oils in use and then also what about blends.

I am principally interested in soyabean and canola which will obviously have different characterisitics but whether the difference amounts to a probelm is not yet known beacuse not all diglycerides will percipitate out and not all monoglycerides will remain in the methanol for any given oil. There may by a 'smoothing out' or 'averaging' to mean that the differences in outcome between soyabean and canola and mixtures thereof may not be overly problematic and a single calculation may do for those oils or oils with quite similar fatty acids compositions.


Sorry Tilly, I edited this as I must remember paragraphs! ;-)


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Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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The feed stock likely has a substantial effect on what is actually dropping out, I doubt an accurate calculation could be made that could be applied to the wide range of WVO out there...

Exactly true. There is a wide variety of VO used to cook a wide variety of products, usually containing a variety of animal fats, and it's used for widely varying lengths of time. The higher the UVO titrates, then the greater likelihood of the dropout test being inaccurate.



 
Location: coldest N.America | Registered: May 03, 2005Reply With QuoteReport This Post
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Originally posted by Dgs:
Jon, you know a lot, anyone that reads your posts can see that.

I have a 400 litre s/steel proc that I have never used.

A few years ago I was going to set it up and do WBD, but never got round to it.

Am I correct in assuming that when using a sealed vessel for the reaction, advantage can be taken to increase the pressure (and therefore temperature) so the reaction is completed in say as little as @ 10 mins, then just carry on with WBD.


Dave is your 400 litre processor designed to be pressurised or is that not what your post is saying?


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Hi Drum,

quote:
Originally posted by Drum:
Now there's an incentive! Are you including yourself? ;-)
Absolutely!
As we speak I am composing an epic Nordic saga describing how the might biodiesel warrior "Drum" struggled incessantly for years with the evil conversion trolls until they at last gave up their vile secret.



quote:
I 'almost' agree with this because it is being used fairly reliably to determine second stage chemical usage but perhaps just not precisely because in its current form the test overestimates the amount of chemical required, so assures conversion.
Exactly the reason to tell people the truth about the Warnqvist test.
If people know the Warnqvist test understates conversion at least they know why they are achieving very high conversion on their second stage and they may want to do some experiments in adjusting the chemical amounts to use less chemicals in the second stage and still pass warnqvist.

When people post that their second stage passed Warnqvist in 10 minutes at 50C, my first thought is "there must have been excessive chemicals in the second stage to pass so quickly"






 
Location: ลึก ประเทศอินเดีย | Registered: March 03, 2001Reply With QuoteReport This Post
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Hello Drum,
I'm glad to see you are very active on here at the moment, even if Troll related.

The 400 litre is known as a 'Grundy' tank. It is designed to run at up to 2 bar and tested to 3.

When my friend used to esterify his ffa's (from cracking glycerol) he did it at 110degs C and at that temp as far as I can remember his reaction was finished in @ 1 hour. I cannot remember the pressure reqd to reach 110degs.

In any case he reduced the reaction time by 4 to 5 hours in comparison to reacting at just under 65 degs.

I'm sure the same will be true in respect of the normal transesterification reaction, in that if it can be done considerably higher than 65 degs then it will go to completion a lot sooner.

My idea was to take a sample and confirm completion, then slowly vent through a top valve so the methanol would flash off and be collected via a condenser.

Now if all the methanol would flash off before any more heat would be applied, I don't know.

Years ago I had one of these tanks set up to reclaim methanol.
I would charge it up with 300 litres of glycerol. It had 2x immersions working from my Genny, running on bio.

The whole process was very inefficient and hardly worth the effort.
 
Location: YORK UK | Registered: April 27, 2014Reply With QuoteReport This Post
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Am I correct in assuming that when using a sealed vessel for the reaction, advantage can be taken to increase the pressure (and therefore temperature) so the reaction is completed in say as little as @ 10 mins, then just carry on with WBD.

I have not tried that myself but I know fabricator was experimenting with increasing the pressure a couple of years ago. I dont recall him posting anything significant with using the increased pressure.
I process at around 70c and and when I WBD I keep the pot temp at maximum 90c so there is not a very big temperature differential between recovering and processing anyways. It processes fast enough so I have not experimented in trying to speed it up.
The only thing that takes a long time is the actual recovery due to the 3/8" condenser tube I used, that was a mistake, I should have used 3/4" or larger. Hopefully I will get a chance to change it out with a larger one this coming season which I hope will cut my recovery time in half at least...
cheers,
Jon
 
Location: Wellington County, Ontario Canada | Registered: February 07, 2008Reply With QuoteReport This Post
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Thanks Jon.
 
Location: YORK UK | Registered: April 27, 2014Reply With QuoteReport This Post
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Hi All. does anybody have any experience of bubbling Nitrogen through oil/bio to dewater? I read about this in a thesis presented here in South Africa. It was only mentioned in passing along with Vacuum distillation.

Drum. That water sensor you pointed me to costs R 7000.00 here so $us 650 or 411 pounds @17 to one exchange rate.
I'm trying to get one on an experimental basis to try. There is a 30 to 40% discount for more than 20 units.

My vacuum processor is stalled waiting for the condenser and wiring and of course some cash.
Finished my 10th batch today so 1800 litres in total to date I am at my break even point for equipment.

Regards Sam
 
Location: Johannesburg South Africa | Registered: October 09, 2012Reply With QuoteReport This Post
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quote:
Originally posted by Dgs:
Hello Drum,


The 400 litre is known as a 'Grundy' tank. It is designed to run at up to 2 bar and tested to 3.

When my friend used to esterify his ffa's (from cracking glycerol) he did it at 110degs C and at that temp as far as I can remember his reaction was finished in @ 1 hour.


If you go the pressure route Dave be safe whatever you do, I don't want you or your processor airborne. The pressure generated is transmitted through all the circuit elements involved including fittings, hosing, hose clips, pump, valves etc.

As a guide, 2 bar will get you to about 85C. At 110C the vapour pressure of methanol is about 5 bar.

Someone quoted a reaction time "rule of thumb" on this forum before stating a reduction in time of 50% for each 10C rise in temperature so using that, the reaction time at 85C would be only 1/4 of the time at 65C. That in itself would be a major achievement.


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Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post



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Originally posted by Sam Sleeman:
Hi All. does anybody have any experience of bubbling Nitrogen through oil/bio to dewater? I read about this in a thesis presented here in South Africa. It was only mentioned in passing along with Vacuum distillation.

Drum. That water sensor you pointed me to costs R 7000.00 here so $us 650 or 411 pounds @17 to one exchange rate.
I'm trying to get one on an experimental basis to try. There is a 30 to 40% discount for more than 20 units.

My vacuum processor is stalled waiting for the condenser and wiring and of course some cash.
Finished my 10th batch today so 1800 litres in total to date I am at my break even point for equipment.

Regards Sam


Sam I am well behind you at only 4 batches and 600 litres. So I have another couple of batches to go to clear me completely but it is a nice feeling to drive past the filling stations for sure!

As pointed out by Tilly my memory is not what it used to be, so could you remind me of the water sensor you refer to.

I cannot help you much with the Nitrogen other than to suggest that bubble drying with Nitrogen will be like bubble drying with "air minus oxygen" so perhaps it is being considered on the basis of it being a way to allay fears of oxidation.


2001 Saab 93 TiD B50
2006 Mercedes C200 CDI (no DPF) B50 (for now)
 
Location: Stroke County | Registered: July 01, 2014Reply With QuoteReport This Post
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Hi Drum. I thought it was you who posted this link. If I'm wrong I'm sure Tilly will remember who posted it.
Any way that is the data I have to date.

http://www.meas-spec.com/produ...-HTM2500B3C4OIL.aspx

Regards sam
 
Location: Johannesburg South Africa | Registered: October 09, 2012Reply With QuoteReport This Post
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