The Imsides method

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

Re: The Imsides method

Hi DavidS

Hi Tilly,

Regarding the testing, my interest is in whether Dr.Mark's method produces a better reaction in terms of a higher conversion due to the supposed drying of the methoxide using cement. To test this I am performing an identical reaction using identical methoxide apart from the fact that one has been "dried" and the other hasn't. To test whether there is an identifiable increase in conversion I will carry out a 10/90 test on each sample.
Best wishes,
David

I await the results of your test.
Just a reminder that when doing comparison testing, to be meaningful, everything between the two tests must remain identical except for the one thing you are actually testing.
In this case it is the drying of the methoxide compared to non-drying.
I eagerly await the results of your test.

I am excited!

[DavidS Junior Member Find all posts View Profile Close DavidS]

Re: The Imsides method

Here are the results of the testing.


THE TEST
1 litre of new rapeseed oil was reacted with 150ml of a koh methoxide made to the Dr. Mark formula detailed on his website.
1 litre of new rapeseed oil was reacted with 150ml of koh methoxide from the same methoxide batch mixed for the above, BUT for this reaction cement was added to the methoxide 24 hours previously and decanted before use..
The ONLY difference between the two reactions is that the second one used methoxide dried by the addition of cement.
The processing starting temperature was 17C. After the addition of methoxide, both samples rose in temperature during the course of the reaction to 23-23.5C . Both samples were shaken vigorously periodically over the course of 1 hour then left 24 hours to settle.




THE QUANTITATIVE RESULTS:


CONTROL SAMPLE
VOLUMES:
The control sample volume at the start was 1000ml of oil plus 150ml of methoxide, so 1150ml
The control sample 24 hours post reaction was 1160ml


The volume of byproduct that settled out was 121ml
The volume of bio produced was 1039ml
This means that the percentage of byproduct formed after this reaction was 10.4%
10/90 TEST
There was a tiny drop of dropout that formed in the bottom of my dropout tube. The bottom of my dropout tube is divided into 0.05ml increments, and so my best estimate of the amount of dropout that formed is .02ml. Its really difficult to be accurate, but it was a really tint amount.




"CEMENT-DRIED METHOXIDE" SAMPLE
VOLUMES:
The “cement-dried-methoxide" sample volume at the start was 1000ml of oil plus 150ml of methoxide, so 1150ml
The “cement-dried-methoxide” sample 24 hours post reaction was 1177ml


The volume of byproduct that settled out was 141ml
The volume of bio produced was 1036ml
This means that the percentage of byproduct formed after this reaction was 12%
10/90 TEST
There was no dropout whatsoever.


TWO QUALITATIVE OBSERVATIONS:


In terms of clarity, 24 hours post reaction, the cement-dried-methoxide sample was bright and crystal clear. The control sample was slightly cloudy and tending towards being opaque
During the 10/90 tests, when testing the cement-dried-methoxide sample, the methanol remained almost clear . The control sample produced a cloudy methanol phase.

[DavidS Junior Member Find all posts View Profile Close DavidS]

Re: The Imsides method

I have posted my results but I have had a message saying that the moderator must approve my post before it's visible

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

Re: The Imsides method

In drying ethanol rather than methanol, a chemistry reference book I have says allow overnight at reflux temperature to absorb all but 0.5% of the water from ethanol. I believe the claim was made that an advantage to this Dr. Mark method was room temperature reaction, without heating. Initially calcium oxide was the material not cement. Calcium oxide is harder to get than cement here. Calcium oxide somewhat forcefully bonds with water removing it from solution, theoretically increasing the methoxide concentration. But if the starting material vegetable oil has water in it the advantage is lost. I don't follow maitrang7995 post. Is that name oriental?

[Tony From West Oz Vice Chairperson of WARFA Find all posts View Profile Close Tony From West Oz]

Re: The Imsides method

The spammer has been removed.

[Tony From West Oz Vice Chairperson of WARFA Find all posts View Profile Close Tony From West Oz]

Re: The Imsides method

I have posted my results but I have had a message saying that the moderator must approve my post before it's visible

David, I don't know why you would get that message, your post has been published at the end of page 3 of this thread with no Moderator intervention.
Tony

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

Re: The Imsides method

Tony, when you say page 3 do you mean page 13. This post of mine is at present the last post on this thread. The results of DavidS arn't showing at the mo?

[Tony From West Oz Vice Chairperson of WARFA Find all posts View Profile Close Tony From West Oz]

Re: The Imsides method

For some reason, the moderation facility did not tell me of a post needing moderation. (I will check this out later) I have approved the post and it shows as post 121 on this thread, at the top of my page 3 (set to show 40 posts per page).
You must have your settings to show fewer posts per page (10?). Post numbers are better than page numbers, I guess.

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

Re: The Imsides method

Thanks Tony, Understood.

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

Re: The Imsides method

Hi David,
Very informative, thank you for posting your test results.

Just curious,
When you made your methoxide did you initially start with one 300ml batch of methanol and stir 30g KOH to the methanol and then partition off 150ml of methoxide for each test batch or did you make the methoxide separately for each test batch?

What did you conclude from your test results?

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

Re: The Imsides method

Very Interesting David, thank you for that. It would be helpful to inform us what actual weight of KOH there was in each of the 150mls of methoxide.

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

Re: Reduced oil temperature in reactor ?

Hi smithy,
In keeping with the spirit of trying to clear up the many inaccurate and misleading posts you have made, I think this is a good point to clear up this amazing bit of misinformation you posted early in this thread.

Anyway just to add, when I tried this method coming up to 3 years ago using Potassium Methoxide dried by using quicklime (CaO) the volume of glycerol recovered after processing was greatly reduced. Glycerol has a variable soap content depending on oil quality, methanol quality and type of catalyst used, but is in the order of 35%. With the dry methoxide there was virtually no potassium soap, so the glycerol volume was about 2/3 of normal.

If this were true, which of course it isn't, that would mean that your byproduct layer (Glycerol) is about 92% pure glycerine.
I have actually pointed this out to you several times over the years but it seemed to make no difference and you continually post these impossible results as being the truth.

If you check the results of the test DavidS has just posted you will see that the byproduct/ glycerol Layer of the batch using dried methanol is actually slightly more than the non-dried batch. Also of interest is the fact that the yield is slightly more in the non-dried batch than the dried batch.
Clearly, the tiny amount of water produced while making methoxide has very little affect on the reaction.

Assuming you really did achieve the results you claim, why do you think your results were so different from DavidS results?

HINT:
While you pretend to be performing a single stage reaction on vegetable oil, you are really performing the second stage reaction on partially reacted biodiesel.


PS:
By the way, I think that DavidS designed a very good test to compare the imsides procedure which dries the methoxide with the a procedure that does not dry the methoxide. I believe his results are valid.
I think both you and Wesley need to have a good close look at how DavidS designed his COMPARISON TEST for your future reference

[DavidS Junior Member Find all posts View Profile Close DavidS]

Re: Reduced oil temperature in reactor ?

Hi Tilly,

i will reply regarding my methoxide mixing a bit later today. I'm just going out to collect some oil.

in fairness, I think if you look at my post #115 on this thread you will see that Dave (Smithy) actually suggested to me the way to run this test on new oil, using the same batch of methoxide and just changing one thing (addition of cement to the second test methoxide). Please give him credit for the scientific method that was applied to this testing.

David

[DavidS Junior Member Find all posts View Profile Close DavidS]

Re: Reduced oil temperature in reactor ?

I calculated the mix for the methoxide as follows:


Dr.Mark's bulk formula calls for 870lites of wvo to be reacted with a methoxide comprising 130 litres of methanol plus 13kgs of KOH.


I calculated that to make 500ml of methoxide to the ratio above I would have to add 50g of KOH to 500ml of methanol.


Once I had got all the KOH to dissolve, I used 150ml of this methoxide to react 1litre of new cooking oil.


I then added cement to the remaining 350ml of methoxide as follows:


Dr.Mark's formula requires 20kgs of cement to be added to a methoxide that contains 130litres of methanol. This calculates to an amount of 20000/13000=0.154g per millilitre. I multiplied this by 350 (the amount of methoxide left in my measuring flask) to calculate that I needed to add 54g of cement.


I added 54g of cement to the 350ml of methoxide and kept giving it a good shake and a stir. I then left it to settle for 24 hours before decanting off 150ml of the clear methoxide from the top and proceeding with the second reaction on a further new 1litre of oil.

[DavidS Junior Member Find all posts View Profile Close DavidS]

Re: Reduced oil temperature in reactor ?

Hi Tilly


You have asked me what I concluded from the test results.


Both tests involved reacting new veg oil with a pretty massive overdose of KOH but an amount of methanol which almost starved the process. I understand from what I have read that consistently successful single stage processes often involve the addition of around 20% methanol, whereas Dr. Mark's formula only uses around 15%.


I observed that the cement-dried-methoxide test produced no dropout and an instantly clear methanol phase during the 10/90 test. The control sample produced a minuscule amount of dropout in the 10/90 and caused the methanol phase to become and remain cloudy.


I concluded from this that adding cement to the methoxide had an observable effect in terms of providing a more complete reaction ( all of course within the limitations of the 10/90 test- let's not start arguing about that again).


I am, however, unable to explain why the control sample produced slightly more bio nor why the cement-dried-methoxide sample produced 12% byproduct and the control sample less at 10.4%.


I would appreciate your thoughts please everyone.