In making, the reaction seems to go smoothly and settles fine however I seem to get soap when washing comes around.

I've even gone so far to just add water and turn it around a little. Same thing and it doesn't seem to separate either. I've made certain that I'm not getting any glycerine, quite certain but still it persists. This after giving 48 hours to settle. Am I not letting it settle long enough or is this the byproduct of an incomplete reaction?

Hello Logan, congratulations on your success!

There are lots of possible reasons for not seperating in the wash.
Was the oil new or used?
Did you do a titration?
How much NaOH total did you use?
Did you shake just once or several times over the hour?
Hard water is more likely to seperate than soft water.

Would like to ask a qustion about the Dr.Peper Method
Titrated at 9+5Base also made a second 11+5
After shaking both they had solids form in them.
Now an 1/2hr later the 9 has 1/3 by-product
11 has 3/4 by-produt.
What can i do to get a better yeild?
More Methonal?

Hello Phild

A titration of 9 NaOH is very high. I am not sure you will have much success with this oil using the single stage method.
You could try to change to KOH and see if this helps.

Is there another way to process this oil i have 20gal heated as we speak?

Hello Phild

An Acid/Base method would probably work

What is H2so4? And where do you get it?
(Thanks for the repleys Tilly)

Hello Phild

H2SO4= Sulphuric acid.
If you live in the US there are some drain cleaners such as "Roebic Drain Flow Blended Sulfuric Acid." is very concentrated.

I'm using new oil actually, I did no titrate but I did overcompensate and used 250/200(on some) 99.5% methanol and 4.9-5.9g of 90% KOH. I've tried variations and still nothing of any noteworthy success, it appears to separate well leaving only a modicum of haze in the would-be biodiesel, however when I get to the wash stage(it's hard water) it appears to emulsify.


In time it will give the appearance that it separates, that is two layers but the "biodiesel" takes on a whitish colour or a lighter hue than what should be expected for an uncontaminated/unused oil sample.

Hello LoganB

If you wish to make ASTM conversion biodiesel from a litre of new oil, tests have shown that 7.8g of 90% purity KOH is required.

Hazy looking biodiesel is normal for just produced and just washed biodiesel.

I've been making BioFuel from virgin oil and have been experimenting with ratios of lye to methanol and at 1.5 times the recommended amount I found that much more of the glycerine settled out. So I went to town and tried 2X the usual amount and had some interesting results.

Corn oil worked best, after wash and drying I had a crystal clear, yellow product. After several weeks of additional settling, there's just a trace of a white film at the bottom of the bottle. Looks good.

Sunflower was also good.

Peanut oil, however is behaving differently. Despite being processed exactly the same, Every wash produces a milky residue, I can't get a clear water to settle after several tries.

It appears to me that it DOES matter the type of oil.

Also, I had made up a small batch of coconut biodiesel using the standard formula and got what appeared to be a good product. However, after sitting for several weeks I have a very clear and looking real good fuel at half of the jug but the bottom half has what looks exactly like a translucent, "cloud" that remains in suspension within the bottom half of clear, seemingly good fuel. This material just floats within the fuel, just like a cloud and has a gel like behaviour if the jug is tilted a bit, to and fro.

I'm making BioFuel for use in model aircraft diesel engines. I've succeeded in running B100 in a two stroke and that means no added oil for lubrication. Correction. Addition of 2% octyl-nitrate was used as an ignition improver.

Even my best fuel has a very small bit of "milk" settled to the bottom after several weeks. Any comments as to what this is and what it means especially the coconut fuel?

First liter trail, very exciting following the Dr Pepper method. After wasing 4 times, water/esthers separate but I ge a layer of white, gluy, milky, yeark looking stuff between esthers and water. Is it soap, how do you get rid of it without loosing to much biod. ?

Hello domdom, congratulations on your success

Allow the biodiesel to settle and do not pour out the middle layer.

If you've got a gluey, white scum, your process was incomplete. Redo it using just 100 ml of methanol and 4 grams of lye in your methoxide solution. Yes, sounds wrong but it works. You'll likely see more "glycerine" fall out. Guess what. That means that the process was incomplete. Your fuel still had a lot of glycerin in it along with methanol and soap.

Before doing this though, do a wash test. Put equal amounts of fuel and water, (ounce or two)in a small bottle, seal and shake. Let sit for an hour and you'll find a scummy, soapy mix. Not good.

Then do a reprocess and try the water test again. You'll likely find better separation of water and fuel with just a layer of white foam in between. This is much better.

Wash your fuel and do the test again. If you still get a layer of white scum, repeat the washing. Repeat until with the water test, you get, within a few minutes, a clear layer of water with a paper thin white layer and pure fuel on top.

My best mix has NO thin, white layer at all.

Next is the methanol test. Add 10% fuel to 90% methanol in a small jar. Shake, and let stand. The fuel should completely dissolve into the methanol. And it should STAY dissolved. Let it sit for a half hour. The best is a pure, CLEAR solution. A SMALL bit of cloudiness is OK but the clearer the better. My best fuel is crystal clear. AND, you should be able to mix any ratios of fuel and methanol and still get a clear solution. My best fuel does that.

This salvages your first try.

Next time, do this. Prepare a small tub full of hot water.

Do your first process as before but after shaking 40 times, set your bottle in the hot water. Let sit, (to keep warm) for five minutes and then, shake again for forty times. Repeat this at least four and better six times. Keeping the solution hot all the while really helps. Replenish your tub water to keep it hot.

A prewash is something that also helps a lot. After your first four shaking's, add 75 ml of water to the mix and do two or three more shaking's. The prewash helps your after wash a great deal. You'll find you can wash a batch with fewer washings.

In the end, you should be able to add water to your fuel, shake the bejeezuz out of it and with ten minutes or so, a Crystal clear water should settle out. When you get there, you have good fuel.

One other thing that can help is to take your newly washed fuel and heat it up in a pot to where it boils as if it were water. Yup, oil doesn't boil but good biodiesel does. This is another test for good fuel. Let boil for five minutes, turn off the heat and let it cool off on its own. This helps to drive off any remaining water and maybe methanol and helps to clarify the fuel. Saves waiting for days to dry out.

When pouring this final mix into your storage container, do so with a funnel and a simple paint strainer. You MAY get some additional "gunk" form that you want to filter out. I don't know what it is, but I'm happy it comes out and I get to keep it out.

Please let us know how you make out doing it this way. Simple is good, but only if it works. And these extra steps are nearly a necessity if you want a good product. With a little practise it gets easy, don't let it intimidate you.

One last point. I had a devil of a time with good fuel clouding over. As it turns out, it was reaching its, you guessed it, CLOUD POINT. That's the temperature at which wax crystals form and that's what the clouds are made of. My shop is in a rather cool basement and accounts for the vexing problems I was having making good fuel.

Good luck.

Hello Andy

Just to clear up a few points.
If a person has an incomplete reaction, it is very unlikely that it will be short by 4g NaOH per litre WVO reacted.
The "Standard" reprocess formula is 1g NaOH/1.4g KOH mixed into 50ml methanol per litre WVO. This formula has been shown to fix most incomplete reactions.
If you do a re-process using your formula and you are using NaOH you will very likely create an immediate gel and will almost certainly produce lots of soap in any event.

I recommend that the first and only test for completion required in most home situations is the WarnQvest Conversion Test (Pat Pend) which you refer to as the Methanol Test.

The other tests you recommend are not nearly as accurate as the Warnqvest Conversion test and the "Boil the Oil" Test is just dangerous.
In my mind, a test where the pot of oil either boils or bursts into flames would not be one of the first 10 tests I would recommend a person to perform.
Have you ever seen a pot of oil heating on the stove suddenly burst into flame? I have, when the oil reaches it's self ignition temperature it jsut bursts into flame.
And Oil DOES boil, at about the same time it bursts into flame.

The Shake-um up test is pretty meaningless. Hard water gives much better results than soft water. It is very good for detecting soap.

Also, just to clear up what you are saying about the "Pre-wash".
The "5% Pre-Wash" is performed at the end of the reaction after you have performed a Warnqvest test and are happy with the test results and you do not plan on any further reactions.
Before the Glycerine layer has been removed add 50ml water to the bottle and give it one more series of shakes.
When the glycerine has settled to the bottom, remove the glycerine and wash as normal.

quote:

Originally posted by Tilly:
Hello Andy

Just to clear up a few points.
If a person has an incomplete reaction, it is very unlikely that it will be short by 4g NaOH per litre WVO reacted.
The "Standard" reprocess formula is 1g NaOH/1.4g KOH mixed into 50ml methanol per litre WVO. This formula has been shown to fix most incomplete reactions.
If you do a re-process using your formula and you are using NaOH you will very likely create an immediate gel and will almost certainly produce lots of soap in any event.


Tilly,
Many thanks for your response. Having asked a few questions in the past and having been ignored on this forum and on another, I decided to do my own experimenting based on much reading. Much of that reading was the sparring going on between competing points of view.

I am making Biodiesel from new oil because I am working on allowing the use of "green" fuel in model airplane, diesel engines. This is a project that I hope to get published in the hopes of exposing the importance and perhaps utility of biodiesel to a wider audience. You might want to review my past posts and links. I am a published author in one of the well established model aircraft magazines and I have some 60 or more engine runs posted on Youtube under the moniker "hopeso". In any event, I can say that reprocessing the way I describe does nothing but produce more glycerine and a more complete reaction. Along with a fuel that washes more easily. The work is not complete, I have stumbled on an intriguing, one off, batch that was re-processed in a way that I didn't document. A fluke but I have a fuel that has characteristics that I'm for now, assuming is extremely good. I'm assuming that because for now, I can't afford professional testing. This is, after all, for toy airplanes. My hope is to create a fuel with a high enough cetane rating so that the addition of ether is not required, as it is in a stock, kerosene based, model diesel fuel. Also, these typically need some 20% or more castor oil for lubrication. I'm speculating that the biodiesel's inherent "oiliness" and lubricity may allow that to be eliminated. That would make a fuel with all combustibles and a "dry" exhaust. No oil sprayed into the environment. I envision a day when model, two stroke engines will be banned outright. If one can be made to run with no oil at all in the mix,,,,

I recommend that the first and only test for completion required in most home situations is the WarnQvest Conversion Test (Pat Pend) which you refer to as the Methanol Test.

Yes, thanks, that is basically the test I am using.

The other tests you recommend are not nearly as accurate as the Warnqvest Conversion test and the "Boil the Oil" Test is just dangerous.
In my mind, a test where the pot of oil either boils or bursts into flames would not be one of the first 10 tests I would recommend a person to perform.
Have you ever seen a pot of oil heating on the stove suddenly burst into flame? I have, when the oil reaches it's self ignition temperature it just bursts into flame.
And Oil DOES boil, at about the same time it bursts into flame.

Very good point, I honestly hadn't thought of that. Many thanks for alerting me and others to that aspect. In fact, you've given me an idea to actually test the self ignition temperature of the Biodiesel I'm making. This will be useful information in the article. Self ignition temperatures are a major issue with our small engines. The lower the better for easier starting and milder compression settings. Yes, I'll do this outside, with a SMALL batch, out in the open and with a fire extinguisher handy.

How the boiling "test" came about was that I followed the Dr. Pepper instructions to the letter. I got a fuel that had a lower viscosity than the base stock and I assumed that I had good fuel. Nothing in the original instructions said anything about washing or testing for good fuel. This was WAY back in the summer. I had trouble getting this fuel to run and thought that perhaps it still had some residual methanol in it. Methanol has a low cetane rating and that would not help at all. At any rate, I decided to heat the batch and as I did I got lots of froth buildup. This appeared to be soap. So I continued the heating till the frothing stopped and I was left with a clump of foam that had body. You could scoop it up with a fork. So I did that and I assumed that this was a good thing to do not knowing any better. And, as I poured out the fuel into a bottle, I realized that some kind of clear gel was going along for the ride. So I used a paint filter and this held most of that back. NOW, I had a fuel that would at least start and run with a GREAT deal of coaxing. That fuel never boiled. As I worked with making more fuel and learned more about the why, hows and why nots, I realized that my first batch of fuel was actually a disaster. But I DID follow the instructions to the letter. In any case, I continued heating fuel to drive off any remaining water not wanting to wait a week or more in this cold climate. And that's when I discovered that the real deal would boil when incomplete fuel would not. So that's my story and I'm sticking to it.

The Shake-um up test is pretty meaningless with Hard water gives much better results than soft water.

This sentence is confusing. Is there a comma intended somewhere and a typo? Are you suggesting that a water test is more accurate using distilled water?

Also, just to clear up what you are saying about the "Pre-wash".
The "5% Pre-Wash" is performed at the end of the reaction and after you have performed a Warnqvest test and are happy with the test results and you do not plan on any further reactions.

Yes, I now realize that adding a bit of water stops the reaction dead in its tracks. Do we want to do that? Don't know, I have made a few litres as described and it's working well.

I'm sure though, that I'm not doing things in proper sequence perhaps and making compensations elsewhere to make it all work,,, somehow. I AM getting good fuels, they pass the methanol test and one passes the water test like gangbusters. But what do I know.

I'm thinking that it may be time to do up a new instruction with all of these issues covered. As in ALL IN ONE PLACE, step by step.

Before the Glycerine layer has been removed.
Add 50ml water to the bottle and give it one more series of shakes.
When the glycerine has settled to the bottom, remove the glycerine and wash as normal.

Many thanks for your response. Despite my crabbiness, I do appreciate your efforts.


Andy

One more point. What fooled me was that I had been given a quart of biodiesel that a local entrepreneur had made from WVO. This material had the same viscosity and oiliness that my first batch had so I assumed that I had done good. After discovering the water and methanol test, I went and tested this commercial fuel and it did not pass.

Meanwhile, I've been lucky enough to locate a source of professionally made biodiesel and test samples are on the way to me. This will be my benchmark for determining if I'm making good fuel.

As for instructions in one place, I realize now, THIS is the thread from where I started. And look how long it's run. Any wonder a guy can get confused with 16 pages of posts to wade through. So it's all there, it seems, just very much diluted over a long period of time.

What would help in any kind of instruction would be pictures to illustrate what to expect.

Lube_Lab_001.jpg (960 KB, 31 downloads) BioLab

Also, an observation that may be regarded as another test.

Take your clear bottle of Biodiesel and give it a vigorous shake. Put it down right quick and observe the bubbles on top. If they dissipate immediately, you've got good fuel. If they take a second or so, still OK. If the bubbles remain and take minutes to disperse, maybe not,

My best fuel, (my assumption based on water and meth test) produces NO bubbles when shaken. None at all. Much like any other volatile, like kerosene, might do. Just a thought.

One more. On the first post of this page, I describe good fuel made from corn, sunflower and peanut oil. None of the above is good fuel. I haven't tested any of it but all have too much viscosity and have a very oily feel. All will be reprocessed as time permits. Right now I'm trying to figure out why I have to reprocess every batch I make. There's the ratio of lye to methanol and then there's the total amount to use per litre. And temperature. And agitation,,, how long exactly.

Got me a cheap blender today. Will try various blend times to see if that makes a difference.

It would be nice, as was the original intent, to simply do the operation in one go and put the damn stuff down to settle and be done with it. Shaking every few minutes for an hour gets stale after a while.

Decanting is a pain. Some devices to help will be illustrated further on.

Hello Andy

I am in a bit of a rush this weekend but have watched your video of a model diesel engine running on B100 and am impressed.

I have done a bit of research. I can not vouch for these numbers, but it appears that Palm oil and coconut both makes Biodiesel with a cetane of around 70.
The down side is that Palm oil biodiesel starts to freeze at around 12deg C

Tallow makes a biodiesel with a cetane of about 75 but the biodiesel freezes around 18deg C.
Biodiesel made from Palm Stearine is said to have a cetane of around 85. I do not know where it freezes.

I will write more later.