The Imsides method

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: Reduced oil temperature in reactor ?

Hi smithy,

One significant point does come to mind here, Wesley only mixed his trial batch for 10 mins at room temperature. I wonder where the 'rule of thumb' of temperature versus mixing time fits in here.

As I read it Wesley mixed and then 13 hours later he passed a 3/27 test.

I do not recall which rule of thumb you are talking about.
These are the two rules of thumb I know of:

"The rule of thumb is that for every 10C the temperature is reduced, the reaction time doubles.
The rule of thumb is that it takes about 1 hour for the reaction to reach completion at 50C." (assuming adequate mixing vigor)
Of course that is for the standard single stage reaction. Perhaps magical procedures are different

I think the really remarkable thing is the fellow on the other forum used only 12% methanol for the reaction and his fall out was 92.5% glycerol

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Just a heads-up.

The only test Mr Imisidies seems to do to judge if he has made biodiesel is that he has drop-out into the glycerine layer.
He does no testing for conversion such as the 3/27 test

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

This calcium oxide use as a drying agent method, seems to have produced a faster reaction at (lower) room temperature of 23 degrees celcius, than a usual one stage reaction at 63 degrees centigrade. The rule of thumb generally is twice as fast for every ten degrees increase in temperature. So 40 degrees increase in temperature would be 16 times faster. I stirred ten minutes then turned off stirring, the methanol did not separate by bouyancy. Enough had reacted so the methanol did not float to the top. I tested using the Warnquest test after ten minutes but used the wrong proportions 10/28 and got 6.1 milliliters of fall out . 13 hours later I found my mistake and retested in a 10/90 Warnquest test and got no fall out. After treating the oil with magnesol and heating to remove water from new corn oil , the reaction was done entirely at room temperature (23 degrees centigrade).

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

This calcium oxide use as a drying agent method, seems to have produced a faster reaction at (lower) room temperature of 23 degrees celcius, than a usual one stage reaction at 63 degrees centigrade.

That is certainly possible, but very unlikely.
When you do some testing that actually shows this increased reaction rate please post it.

I stirred ten minutes then turned of stirring, the methanol did not separate by bouyancy. Enough had reacted so the methanol did not float to the top.

Methanol does not separate out and float to the top after you begin stirring- even after one minute.

Passing the 3/27 test 13 hours later only shows that the reaction can be performed at room temperature but that was never in question. Everyone already knows that.

Just because you stopped mixing after 10 minutes does not mean the reaction stopped.
That is why, in an earlier post to this thread Tony said:
"Question: How would you stop the reaction of a sample so that the time since taking the sample does not impact oh the conversion rate?"

You do not know when the raction reached completion other that sometime within that 13 hour time frame.
You also do not know how long it takes for your reaction setup to make biodiesel using the standard single stage method.

While it is a rule of thumb that the reaction generally takes about 1 hour at 50C for backyard reactors, as smithy has demonstrated, some reactors are quicker than others.
Small test reactors have been shown to typically be quicker than the large backyard production reactors.
Back in the early days of biodiesel production when it was common practice to make test batches in blenders, it was quickly recognized that the blender reaction went very fast.
Every reactor is different and takes a different amount of time to perform the reaction.
We need to know how fast your reactor is.

You need to design a comparison test between the Standard single stage method and this imisides procedure to demonstrate whether there is a meaningful difference in the speed the reaction goes.

If you need help in designing this test please let me know. I have designed many biodiesel tests over the years

At this point all you have demonstrated is that you do not need to heat to achieve a complete reaction, but everyone knows that already.

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

Tily a mistake in your debate is that in general for every 10 degree increase in temperature the reaction rate doubles (for similar organic reactions). Introducing the inorganic drying agent into the mix is cheating, since it shifts the methoxide production (equilibrium) to the right making it a different rate equation (that's calculus). I'm sorry I forgot the quiestion.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

Tily a mistake in your debate is that in general for every 10 degree increase in temperature the reaction rate doubles (for similar organic reactions). Introducing the inorganic drying agent into the mix is cheating, since it shifts the methoxide production (equilibrium) to the right making it a different rate equation (that's calculus). I'm sorry I forgot the quiestion.

I am not debating anything.
I am waiting for you to do some meaningful comparison testing that will show whether this procedure works as it is claimed to and is actually better than the standard single stage method.
Right now you are just guessing as to what might happen.

I eagerly await the results of your comparison testing.

[Dr Mark Senior Member Find all posts View Profile Close Dr Mark]

Re: The Imsides method

Please note that I have now set up a link on my website devoted to this method. http://drchemical.com.au/biodiesel Note to moderators - this is not a commercial site, and all the information is freely available. Can i also suggest tha tthis method be included as a sticky (perhaps just "Room Temperature Method" or something) - at last it seems that people are starting to wake up to the fact that heating your biodiesel and doing titrations is not necessary.

One of the problems with the infopop forum was that there was a limited amount of text available, so I had to abbreviate things a little. But on my own site I had no such restriction of course.

The first section lays out the chemistry of the process, and the second takes you through the method. You do not have to understand the chemistry of the process to follow the method.

Also, please note that I will not be making any further contributions to this thread. Firstly, I do not have time to conduct online chemistry tutorials, and secondly I do not have the time or patience to correct the errors of the self-styled experts on this forum who have no formal training in chemistry and just confuse people with their misconceptions and poor advice. This method involves concepts for which you would have to have studied organic and physical Chemistry at tertiary level to understand. If you haven't done that, don't expect to understand the chemical principles.

My website lays out the process and the chemistry in detail, so all these questions will be answered there. For those of you that are students of Chemistry I can help you understand some of the finer details if you wish, but for the rest of you, just follow the process as laid out and it'll work. The beauty of this method is that all the quantities are bulk quantities, and there are no fiddly titrations or exact weighing required.

Also there is a place at the bottom where you can ask questions or make comments, and I will respond accordingly.

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

At 3:25 PM today I put 100 ml new methanol and 4 grams 85% potassium hydroxide and 2 grams anhydrous calcium oxide into a 500 milliliter round bottom boiling flask. Stoppered the flask. Did magnetic stirring on the flask for 1 hour, allowing the calcium oxide to adsorb water. At 4:29 PM put 325 milliliters of Magnesol treated new corn oil into the methanol with fast magnetic stirring at room temperature. Room temperature is 22 degrees celcius. At 4:39 PM did a 10/90 test, I got 0.6 milliliters of fallout most of which appears to be a white solid. At 4:58 PM did the 10/90 test again, there was 1 ml of solid white fallout (calcium oxide solid). Within 30 minutes all the corn oil seems to be reacted at room temperature.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

At 4:39 PM did a 10/90 test, I got 0.6 milliliters of fallout most of which appears to be a white solid. At 4:58 PM did the 10/90 test again, there was 1 ml of solid white fallout (calcium oxide solid). Within 30 minutes all the corn oil seems to be reacted at room temperature.

I do not know how you came to this conclusion.

One time you had 0.6ml of unknown fallout in the 10/90 test and the next time you had 1ml fallout in the 10/90 test. You reacted 325ml of corn oil.
That would mean you have a total of between 19.5ml and 32.5 ml of fallout in the entire 325ml of new corn oil reacted.
That strongly suggests there is a lot more than just the 2g of calcium oxide initially added to the reaction in the fallout
What was the weight of the 0.6ml of fallout?
How did you determine there was no oil in the fallout?
It seems you are just guessing/ hoping there is no oil in the fallout.

PS You are supposed to remove the calcium oxide before you do the reaction.


A quick look at the chemical quantities used in the reaction

Per litre of new corn oil your chemical quantities for the reaction work out to:
12.3g KOH per litre of new corn oil
308ml methanol per litre of New corn oil
That is certainly a huge excess of chemicals and you should have no problems achieving a complete reaction at room temperature using the standard single stage method.

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

I initially intended to determine if a reduced temperature for the transesterification reaction was practical. An excess of chemicals was not my concern. It may be a different order of rate equation (a calculus chemistry thing). I have reacted biodiesel for an hour at 63 degrees centigrade in the past (just under the boiling point of methanol at atmospheric pressure) without a proper 10/90 test. I've read that calcium soaps are a problem with this Imisides Method, so I removed the free fatty acids and most of the water to minimize the formation of soaps via neutralization and saponification reaction. My biodiesel from my last experiment still had a little glycerine falling out and it's a little cloudy from calcium oxide powder and calcium (di) hydroxide suspended in the bio. I'll vacuum filter it down to 1 micron (1 micron filter paper) maybe tomorrow.

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

I initially intended to determine if a reduced temperature for the transesterification reaction was practical.

Describe what you mean by practical.
People have been doing the reaction at room temperature for years. Room temperature reaction is only something new to you and imsides. Everyone who has any real knowledge about producing biodiesel knows the reaction will go at room temperature.
That is a given

I've read that calcium soaps are a problem with this Imisides Method,

I have read a lot of nonsense posted about this procedure. As far as I can tell people are just making it up as they go along without performing any meaningful testing to support their amazing claims.

so I removed the free fatty acids and most of the water to minimize the formation of soaps via neutralization and saponification reaction.

What did that entail- this is the first you have mentioned "removed the free fatty acids and most of the water"

it's a little cloudy from calcium oxide powder and calcium (di) hydroxide suspended in the bio.

Explain how you determined the cloudiness was "calcium oxide powder and calcium (di) hydroxide suspended in the bio?"
As far as I can tell you are just guessing again

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

Magnesol advertises purifying vegetable oil in restaurant settings, extending its' usable good quality life. It absorbs polar moilecules which free fatty acids are. I boiled off water from the new corn oil, I saw bubbles forming. There is a principle in chemistry (except radioactive chemistry) that no new elements are formed, there is a continuity of material. New molecules might be formed but the material you started with are the amount of elements you ended with in an experiment. You consider what was present then I see cloudyness in the biodiesel. What could it be? There's a limited number of possibilities. It's not radium, francium uranium etc since they weren't present initially. It might be calcium oxide and calcium (di) hydroxide as one was present and one is an expected product present in the biodiesel. If that's a guess?

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

I boiled off water from the new corn oil, I saw bubbles forming.

Really?
I do not recall ever seeing water boil out of new veg oil

You consider what was present then I see cloudyness in the biodiesel. What could it be? There's a limited number of possibilities. It's not radium, francium uranium etc since they weren't present initially. It might be calcium oxide and calcium (di) hydroxide as one was present and one is an expected product present in the biodiesel. If that's a guess?

I see cloudiness every time I make biodiesel.
It is not radium, francium uranium etc since they weren't present initially.
I guarantee you it is also not calcium oxide and calcium (di) hydroxide.
You are just making guesses as to what it might be and presenting them as fact.

That 2g of calcium oxide you initially added to the reaction sure seems to have gone a long way

[WesleyB Donating Member Find all posts View Profile Close WesleyB]

Re: The Imsides method

I used a magnetic stirring hot plate with magnetic stir bar in a 2000 milliliter beaker using moderately fast stirring at atmospheric pressure . I heated the new Wesson corn oil up to 105 degrees centigrade. What would you assume bubbles forming and floating to the top were? Maybe water? That's a (educated) guess. You just assume new Wesson (name brand) corn oil is completely dry (anhydrous). It's not. I think you are guessing that I'm guessing, I'm not. Kind of hard to explain that one. In producing synthetic fuel energy input is an important question. How much energy does it require to make a manageable liquid fuel to run an engine? For example I made about 100 grams of biodiesel from acorns, but I spent $20 twenty dollars American in acetone to extract the vegetable oil from the ground acorns. A fast transesterification reaction at room temperature is potentially profitable industrially. This reaction at room temperature and it's fast is significant (probably). Tilly do you actually make biodiesel or are you an arm chair intellectual observer?

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: The Imsides method

Hi Wesley,

What would you assume bubbles forming and floating to the top were? Maybe water?

It may be water. I have never seen new veg oil bubble when heated.

You just assume new Wesson (name brand) corn oil is completely dry (anhydrous). It's not.

I do not recall ever saying that I thought Wesson brand corn oil is completely dry (anhydrous)

I think you are guessing that I'm guessing, I'm not. Kind of hard to explain that one.

Without any proof you posted that your biodiesel was: "a little cloudy from calcium oxide powder and calcium (di) hydroxide suspended in the bio"
Without any proof you posted: "At 4:39 PM did a 10/90 test, I got 0.6 milliliters of fallout most of which appears to be a white solid. At 4:58 PM did the 10/90 test again, there was 1 ml of solid white fallout (calcium oxide solid)"
Without any proof you posted: "Within 30 minutes all the corn oil seems to be reacted at room temperature."
Posting something as being a fact without having proof is guessing.

Tilly do you actually make biodiesel or are you an arm chair intellectual observer?

Unlike you, I actually make and use biodiesel for my everyday driving. Over the years I have made squillions of litres of biodiesel.
In fact I will be starting this years production in a couple of weeks while my wife is visiting the USA

Of course it goes without saying that I am also an intellectual observer