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Tilly
03-13-2006, 10:10 PM
Hello BiggestDawg, welcome to the forum and congratulations on your success!

Drano is not 100% NaOH and it seems to vary between 40- 60% so perhaps 1.5 level Teaspoons would be in order.
The amount of glycerine being about the same as the methanol used is only a rough estimation.

KOH (Potasium hydroxide) can be used in place of NaOH. It apparently disolves quicker in methanol and the glycerine layer remains liquid instead of solidifying.

pickledtoad
04-01-2006, 03:48 PM
I am getting ready to do my first small batch and am gathering upo the supplies and have a quick question.... does the bottle have to be glass and if so where migght I find one good enough

makenamicro
04-02-2006, 06:40 PM
Where can I find a current working link discribing the Dr. Pepper Viscosimeter?

Tilly
04-06-2006, 01:52 AM
Hello pickeledtoad
The reaction bottle does not need to be glass, PET works fine.

Hello makenamicro
Look Here. (http://biodiesel.infopop.cc/eve/forums/a/tpc/f/419605551/m/590108381/r/590108381#590108381)

mastermute
05-11-2006, 07:44 PM
Hi!

I just made my first "Dr Pepper" batch of BD, and I'm impressed! Thanks for the great instructions!

I have a small issue with my experiment though;
It says over at http://www.biodieselcommunity.org/makingasmallbatch/ : "Typically the glycerine layer is about the same or a bit more than the amount of methanol used." and my estimate is that I have half the amount (or less) of glycerine (glycerol?) compared to the amount of methoxide I put in.

My simple question is : What can this mean?

(
EDIT:

Some further facts that I think might be useful to find a source for the problem (as I have looked around elsewhere too for the solution)

The lye I used says 85%-100% NaOH (I use it successfully for soapmaking)

I used "half a teaspoon" of lye, which isn't very precise.. I "eyed" half a measurment of a teaspoon measure that said "1 Teaspoon (5ml)".

I can't say that I felt the mixing of the methoxide was "exothermic". I cound't feel a "significant" temeprature raise, not like the one I feel when mixing [the same] lye with water for soapmaking (But the soapmaking uses a significantly larger addition of lye).

)

Tilly
05-11-2006, 10:12 PM
Hello mastermute, congratulations on your successful batch of biodiesel

The "Glycerine layer" amount will vary. With new oil it will be less than with Waste oil. These measurements are only rough approximations.

I have not seen NaOH less than 99%. If you have 85% NaoH you will need to increase the base amount of NaOH from 5g to 5.9g.
If you use the same NaOH in the titration as you use in the reaction you do not need to adjust the titration amount.

The Teaspoon measurement is only there for poeple who do not have accurate weighing equipment.
Methoxide does not contain the same amount of NaOH as the water soap is made from and will not heat up as much.
Also for the small amount of methoxide you made, most of the heat would have been "used up" heating the container a few degrees.

mastermute
05-11-2006, 10:30 PM
Thanks a lot for that quick answer!

I used NVO so that might be the reason then...

I'll do a new batch tomorrow as I managed to make a soap/BD emulsion due to not reading the instructions for washing properly... http://biodiesel.infopop.cc/groupee_common/emoticons/icon_rolleyes.gif That'll teach me to go to bed earlier!

Again, thank you for showing me the way to make BioDiesel! I hope more people discover how to make fuel from renewable sources.

bjornen11
05-15-2006, 02:04 PM
I am trying to start making biodiesel. I have good used oil (titration = .1) but when I make liter batches, and then do a water test for quality, it always makes soap. I'm using 1 liter oil, 250 ml methanol with 6.1 grams KOH dissolved in it, shaking for 10minutes, letting settleat least 24 hours. Settles well, but the fule part is not crystal clear (can't read through it). iS it possible methanol is bad, does it go bad? I don't want to make larger batch until I can make a good liter batch. Not sure what to try next.

Tilly
05-15-2006, 07:31 PM
Hello bjornen11, welcome to the forum

The "Shake-um up" test is meaningless as a test for quality. It is just more crapola misinformation posted on the JTF misinformation site.

The base aount for KOH is 7 adjusted for purity, not 6.
Also, if you are doing the reaction at 50deg C you should re-mix several times over an hour for maximum conversion.

imported_Bio1Ak
05-16-2006, 11:20 AM
Hi Tilly. If the JTF "shake-em-up" test is garbage, than what is the proper test for quality?
I tried making two test batches, one with wvo and one with new soy oil. We used Muel Kick sodium grainuals and Heet (yellow). Tested the wvo and used 9.5 grams, 3.5 for the soy. The wvo made creamy mayo floaters and the soy made a thin milkshake. (shake-em-up test) I am not about to try and put this stuff in a motor if it does not pass some sort of test. Do you have a good test proceedure?? Thanks in advance.

Tilly
05-16-2006, 11:59 AM
Hello Bio1AK

The chemical reaction for biodiesel production isvery dependable and repeatable.
Follow the correct procedures and you will make high conversion biodiesel.

Also, be aware that the correct formula for making ASTM conversion biodiesel is at least 5g NaOH+ titration mixed in 200ml methanol

The only "Backyard" Test for conversion that I am aware of is the World Famous Dr Pepper ASTM Reprocess Test (http://biodiesel.infopop.cc/eve/ubb.x?a=tpc&s=447609751&f=419605551&m=435107459&r=435107459#435107459) (Pat Pend)

ACorder
05-29-2006, 10:09 AM
Hey, just tried my first batch using Dr. Pepper method the other day, using 4mg/NaOH in 250 ml of Methanol - everything seemed to settle out nicely, but never cleared stayed cloudy - washed it after a day til water was clear, BD remained cloudy, now after drying for a day there is a separation layer - cloudy BD on bottom and a thin layer of clear liquid on top - any suggestions on what this is?

Tilly
05-29-2006, 03:23 PM
Hello ACorder, congratulations on your success

The top layer is probably the meniscus of the biodiesel.
Are you drying it in the sun with the top off?
You could just pour the biodiesel into a sayce pan and heat it to around 100deg C and it should clear.

rjr311
06-06-2006, 02:22 AM
I did this this weekend and when I added the oil I saw a seperation-like activity. Shook it up and then shook it up again a few times.

I have 2 liters of brown liquid with some coagulant looking stuff at bottom of container but not completely seperated.

I think my lye "Rooto" 100% Lye which is the replacement to Red Devil may have been opened. Does this sound like my mixture of methanol and lye may not have been as full strength as it should have been ?

Is there anything I can do to re-attempt the process with the current solution ?

Thank you -robert

Tilly
06-06-2006, 04:08 AM
Hello rjr311, congratulations on your first successful batch of biodiesel

Can you be more specific as to what you mean by
"coagulant looking stuff at bottom of container but not completely seperated."

How do you know it was not complete seperation?

rjr311
06-06-2006, 12:32 PM
when I poke the bottom layer it seems to be like thin pudding. I can scrape the sides of the bottle like I was cleaning a dirty aquarium and the gunk on side of bottle drops to bottom ( it so think I can not tell ).

I had 2 sources - one unused cooking oil the other used asian restaurant oil.

The virgin oil seperated into
15-20% clear yellow/gold solution ( BioD
70% cloudy yellow/gold solution ( ???? BioD ????
< 10% darker gold on bottom ( glycerine

Looked great.

The used oil 2 days later is all dark-ish with a semi-solid layer on the bottom which can not be seen through and a possibly less denser layer on top. This seems to be about a 50/50 volume ratio.

imported_Penguy
06-19-2006, 12:03 PM
Hi Tilly,
I am still a newbie. Working about 100 liters at a time. I just did a test shake in a small bottle of some dryed bio. 12 hours later it has separated but I have thin layer of what looks like emulsion between very clear colorless water and bio.
1. Appleseed processor, at 120 F, pump 2 hours.
2. Have 200L settling tank, let settle for more than 24 hours. Good separation of bio and glycerine.
3. Heated wash tank at 96 F. Mist wash 2 or 3 times depending on how clear the wash looks.
4. Bubble wash until wash is clear, what ever it takes. Have lots of water and easy disposal.
5. Bubble dried for 12 hours overnite.
6. Bio is crystal clear when I put sample in liter bottle and added 75 F tap water. I shook it hard for several seconds. More than 10 but not 30 seconds.
7. Separation was apparent in 10 minutes. 12 hours later I have crystal clear water with soapy emulsion like layer between water and bio. I guess the layer is 2mm thick. The water is clear with no disolved or suspended material.
8. Sorry I forgot. My oil is soy and comes from a chinese restaurant.

Does this appear to be acceptable bio? Am I being too much of a perfectionist? I wanted a perfect split.

One more data point. My house tap water pH is 7.4+, the water via hose to my wash tank is 8.3-8.4. The wash water when clear is 8.3. This is well water and what I get is what I get.

I am having a little frustration. I live in Maine and have about a 3 month window of warm weather to process my fuel. So far it has been pretty slow production.


Thanks again for your wisdom.

Tilly
06-19-2006, 12:42 PM
Hello penguy

What were the quantities of reactants per litre WVO?

imported_Penguy
06-19-2006, 05:00 PM
Tilly,
Sorry to be slow to get back. We are building a home in the forest.

11g KOH and 220ml methanol per L of WVO. (In a 97.5 L batch of WVO I use 21.5 L of methanol, for this run I used 1073g KOH, and I also use 13.2 L of glycerol.)

From the forums I read where the use of 10% glycerol helped the production.


Once again thanks for your expertise. I must be on the back side of the clock for you. I'll check back in a couple of hours.

Tilly
06-19-2006, 10:14 PM
Hello Penguy

The glycerine should not be left in the oil when it is reacted.
The only reason for using glycerine before the reaction is to clear some of the crud out of the oil.
If you do use glycerine this way you need to remove it from the reactor before the reaction or some of your methoxide may become tied up with the glycerine and not used in the reaction.

If your oil titrated 3 or less KOH and you do not leave the glycerine in the reactor, you should get a very good reaction.

imported_Penguy
06-19-2006, 10:59 PM
OK Tilly,
I will drop the glycerine out of the mix.

I do not have anything on hand to test for soap, that stuff is in the mail. I can wash some more or do I need to reprocess this current batch? Or should I just fuel up with the current batch? Now at almost 24 hours there is still some residual foam or emulsion still left at the bio water interface. Any feelings about this?

Should or can I send a picture as an attachment?

And then I will leave you in peace.

Thank you.

Tilly
06-20-2006, 12:35 AM
Hello penguy

I use my eyes to test for soap.
If the wash water is cloudy there is soap present.
If the wash water is clear there is not much soap present.

If the biodiesel is crystal clear at the lowest temp it will experience it is ready to use.
You can not visually determine the conversion of the biodiesel by looking at it.
What type of engine are you using the bidoesel in.
I would personally use the biodiesel but that is finally for you to decide.

imported_Penguy
06-20-2006, 04:56 PM
Hi Tilly,

Done. I rewashed it overnite. Almost dry again. I will burn it (Oops, drive it). Several diesels, 2000 Jetta TDI, 97 Dodge Cummins, then generators, saws. etc.

Thanks again for all your help and advice.

grandpa
07-24-2006, 12:43 AM
Hi Tilly, thanks for all the BD info. I am a newbie and tried the Dr. Pepper processing technique. I am using waste restaurant oil. I titrated it at 4.5 Ml. I heated oil to 60 degrees C., added methoxide mix of 10G NAOH and 250 ML of yellow HEET. I shook mixture about 40 shakes. Then shook it again 10 minutes later and let it sit. I ended up with three layers. Top layer is golden yellow (Not clear) middle smallest layer is whitish jellow like, bottom layer is dark. I thought the top layer was the BD and the bottom layer the glycerol. I don't know what the middle jellow like layer is. Soap? Any ideas? How would I get rid of besides draining it away. Thanks for all the help!

Tilly
07-24-2006, 08:03 AM
Hello grandpa, welcome to the forum and congratulatios on your first successful batch of biodiesel.

Are you from Allentown Maryland? I used to go to the Tayac Elementary school in Allentown!

I suspect the middle layer is soap.
It may have some biodiesel tied up with it so you might try to wash it very gently.
Please keep us informed.

Keith Ohls
07-26-2006, 08:01 PM
tried my first small batch after four hours no seperation yet. when I put in the methoxide it boiled. should it have done that? I used new oil. heated it to 140 F. I did not see any color change.

Tilly
07-26-2006, 10:30 PM
Hello Keith

If the methanol boiled you have lost at least some of it. this is not a good thing.
140f= 60C which should not boil the methanol. Possibly your thermometer is inaccurate.

Keith Ohls
07-28-2006, 03:19 AM
I will get a new thermometer also when i put the hot oil into the plastic bottle it melted the bottle. I then went and bought a glass bottle. but now i would like to make a batch about 4 X as big. do i just multiply by how much more i want to make. the amount needed for the dr. pepper one ltr thanks for the help one day i hope to be makeing enough for my tank
Keith

Tilly
07-28-2006, 06:01 PM
Hello Keith

Did you go to 140deg F or C?

Yes, just multiply everything by 4.

Fuzznag
07-29-2006, 06:54 PM
Hey Tilly, just been browsing a Lister engine group on Yahoo and noticed that recent threads are questioning the Dr Pepper method (and you personally).

posted on http://groups.yahoo.com/group/Lister_CSOG/message/1524 27 July 06
RE: [Lister_CSOG] Dr Pepper method for biodiesel?


It's a hokey soda bottle shaker method that doesn't make very good
biodiesel. It's cool for doing demonstrations. We were using it in classes
long before the "inventor" heard about our demonstrations and decided to
claim the process, without understanding the caveats..

Steve Spence

Director, Green Trust

http://www.green-trust.org

Any body else find "it doesn't make very good
biodiesel" I have never had a problem with quality.

Reading a bit further it seems like Steve Spence holds Keith Addison in high regard so that probably says enough about him so should be ignored.

Just thought you may be interested in what was being said in other places, I guess others may have seen it.

Fuzznag
07-29-2006, 07:24 PM
yeah, that's what I thought

Tilly
07-30-2006, 11:38 AM
Hello Fuzznag

That is my good mate steve Spence,
He used to be Keith Addison's right hand gofer in the USA until Keith found out he was a republican and run him off his forum.
For a thumbnail sketch of Steve's relationship with me look here. (http://biodiesel.infopop.cc/eve/forums/a/tpc/f/649605551/m/879607261?r=702105426#702105426)

rhea530
08-02-2006, 04:23 PM
what is the shelf life of biodiesel? any special requirements; container, dark room, ...?

jim95437
08-14-2006, 03:44 PM
Hello;
Yesterday I made my first batch using this formula. I used 1 liter of wesson oil, 250 ml of Heet Methanol, and 100% lye (NaOH), Rooto brand, 1 Tblsp (not 1 Tsp). I shook violently for 1 minute (I don't know why).
10 minutes later I had 1 inch of clear dark amber fluid on the bottom and light Cloudy mixture on top. An hour later the line separating the two layers got irregular (lumpy) and two hours later there was glop on the bottom, about one inch and about one eighth of an inch of dark amber liquid then the rest cloudy mixture.
This morning what I found is one inch or so of glop on the bottom and beautiful light clear amber liquid on top. maybe a little more than a liter.
My question is this: Is this biodiesel ontop, and is it worth washing. I am assumming that the bottom layer is soap, glycerine and methonal.
Any feed back would be appreciated,
Jim

Tilly
08-17-2006, 04:02 AM
Hello Jim, welcome to the forum

Congratulations on your success. Yes, it is biodiesel.
You have certainly made extra soap from the excess NaOH but just wash the biodiesel and it should work fine.

Ash786
08-17-2006, 10:30 AM
Hello & thanks for this technique.

I am fairly new to biodieseling and to be honest originally was a little confused with the amounts of base to use 3.5 or 5. This was mainly cos my first source of learning info was the JTF website but have now become a true convert!

Anyways I have mainly been using some WVO, hydrogenated vegetable oil and using at least 25% methanol and 6.5g NaOH for processing which turns out just fine.

Recently, I got some WVO from a different source which was really thick and black, like engine oil. Titrated to 5 so used 10g NaOH and 25% methanol and processed as usual for 90mins and did the 5% prewash. When I took a sample out, I could not see any seperation, the sample was just all black! After about 15mins, I started getting agitated so started shining lights in all angles trying to find seperation. And lo and behold I found it, clear distinct seperation with looked like really dark soot as the glycerin layer and kind like a blackish red ink layer of what I assumed to be biodiesel.

So as the seperation could be seen all be it with a light I finished the washing drying and decided to put some in my car, even though it was slightly thicker then my normal biodiesel. I had put 20litres of this "biodiesel" in with about 40litres of the good palm biodiesel in my vehicle. Immediately I got problems with my car choking and going off with plumes of white smoke.

It had difficulty starting and when it did, it would chuck out smoke and go off. On opening the filter there was kinda bubbles at the outlet of the fuel filter. I changed the fuel filter to a new one but the same problem so i decided I had no choice but to pump it out. I must of pumped out about 30 litres and then added 20 more litre of my usual biodiesel before my car started to get better but even then it was starting and stopping so I had to put in 20litres of normal petrodiesel before it started running normally.

Any ideas as to why this oil was so dark and why I had problems with it? The other main difference I noticed was with this oil when I was transferring for washing from my processor tank, there were large jellyfish like formations at the bottom of the processor tank which I assumed were soap. Don't normally get these with the palm oil I use.

Could there have been alot more water than I thought in the oil before processing? Which may have under-reacted the oil during processing by taking away some of the NaOH from the main reaction and using it to make soap instead. The symptoms of my vehicle, are they what you'd expect if there is water in the biodiesel used?

The reason, I ask is that although I had vowed to never use that source again, it could well be that I may have a good source of WVO (400litres a month) if I figure out what went wrong and process better.

Many thanks in advance.

jim95437
08-17-2006, 12:33 PM
Hi Tilly;
Thank you for responding. I went ahead as if it were BD and washed it. I think I lost almost half of my yield in the process. Took ten washings. What I have now is a very pale yellow, somewhat cloudy BD, about 600 ml I would say. That is from 1 liter of oil. So It is now in an open mouth mason jar and i'm not sure how to dry such a small amount or quality test it. Any ideas?
Jim

Tilly
08-17-2006, 12:40 PM
Hello jim

Don't worry about quality testing, you have used plenty of NaOH so should have achieved good conversion.

You can either leave it sit in the sun for a few days or pour the biodiesel into a pan and heat on a stove to 100deg C. Make sure you stir while heating to avoid "Bumping"
The biodiesel will almost certainly be clear at this temp.
You will probably notice water puddles on the bottom of the pan.
Decant the biodiesel into a dry non-plastic container and allow to cool. If it turns cloudy as it cools re-heat to 100deg C and it should stay clear this time.
The biodiesel is now ready to use.

Tilly
08-17-2006, 12:43 PM
Hello Ash

I suggest you start a new thread with your question. I have not experienced what you described but I bet there are people who have.

jim95437
08-17-2006, 12:47 PM
Hi Tilly;
It looks like we are on the computer at the same time, Thank you for all your help. I will dry as you suggested. I am going to make another small batch with WVO this time. and am getting very exciited about all this. Thanks again,
Jim

Ash786
08-17-2006, 03:38 PM
Thanks Tilly.

Will start a new thread and see what I can learn from others experience.

jim95437
08-19-2006, 01:32 PM
Hi Tilly:
I just wanted to add one more note for the sake of completion. When I came home to dry as you suggested, the BD was a light amber in color, comletely clear liquid. I could very easily read a letter through it. Just putting it in the wide mouth jar allowed it to dry overnight. I have ordered some lab equipment and will make a batch of WVO BD next. Thank you for your help.
Jim

Radical53
09-17-2006, 06:53 PM
I am a newbie at making biodiesel and was wondering what is the perfect consistency of Bd and can you put Bd in a gas tank that alredy has dino diesel in it.

Tilly
09-18-2006, 12:09 PM
Hello Radical53, welcome to the forum

The perfect consistency is ASTM (or DIN in a pinch).
Mix and match in all proportions

DarylF
10-05-2006, 06:03 PM
Hi all. 1st time bio-d person here and I've just messed up 2 litres of store bought oil.

I cant really say whats gone wrong I hope you can.

1st litre, 10g KOH into 250ml of Methane, totally disolved. Poured into the 50-60c warm oil. Mixed the thing like crazy since I believe in that, good 50-60 reversals of the bottle then left to settle. Almost immed. the glycerine started to settle but it only went down 3cm then stopped!!!

2nd litre, 15g KOH and everything else the same and it didn't start to separate at all!

Used more KOH than listed for NaOH since I read you need 1.4 times KOH than NaOH.

Whats gone wrong????

Thanks,
Daryl

dodgeram
10-05-2006, 06:15 PM
Try it with 8 grams Koh and 200ml methanol and you should get better results . With 250 ml methanol it is likely that the excess methanol is keeping the glycerine in suspension . I have had this happen before and got the glycerine to settle by evaporating the methanol out of the batch . Do not try to evaporate methanol inddors though .
Good Luck ,
Shannon

Tilly
10-05-2006, 10:55 PM
Hello Daryl, welcome to the forum

Yes, I have seen that with high amounts of KOH.
Add about 50ml water to the two batches that did not seperate and give them 40 good shakes.
I bet you get seperation.

DarylF
10-06-2006, 09:22 PM
Hi guys.

Thanks for responses. Actually by morning both had settled and I can tell you one thing the high KOH batch is clear and wonderful looking! The 1st one is still cloudy and doesn't seem to want to clear.

I made a 200ml methanol and 8g KOH batch as you suggested but its looking just like the 1st batch, staying cloudy but yea reaction and settling out of the glycerine happened much faster.

But wow the high (15g) KOH batch looks great! Why is it so clear and the 10g and 8g KOH batches stay cloudy?

Also could someone please post links that you think are good for the how2s on titration and for the washing of the BD?

Thanks,
Daryl

PS Well done for making posts editable!

Tilly
10-07-2006, 09:48 AM
Hello Daryl

For the easiest method of titrating you can not beat the World Famous Chopstick Titration Technique (http://biodiesel.infopop.cc/groupee/forums/a/tpc/f/719605551/m/9541092001) (Pat Pend)
For the easiest method of washing your mini-batch of biodiesel, you can not beat the World Famous Dr Pepper Wash Technique (http://biodiesel.infopop.cc/6/ubb.x?a=tpc&s=447609751&f=719605551&m=741607061&r=741607061#741607061) (Pat Pend)

AndyW
10-26-2006, 04:07 PM
I'm new to The Biodiesel game and my interest is its use as a model airplane fuel. I've managed to run a small, two stroke diesel engine on ALL Biodiesel,(no added lubrication)with just 2% of an ignition improver made by Amsoil called a cetane booster. I don't believe it really boosts the cetane number, just that it improves ignition thus allowing the engine to respond to the fuel as IF it had a higher cetane number.

At any rate, I'm experimenting with various fresh oils such as olive oil. Can anyone advise if one type of oil or the other might be better suited to my uses.

I've also tried to biodiesel coconut oil. Yes, this is an EXPENSIVE Biodiesel if you use it in you 500 HP Mack truck but this engine has only .15 cubic inches capacity. Even then, this is only an experiment.

Right now I've got a fresh batch of olive oil and coconut oil sitting to allow as much gunk to settle to be drained off. Yes, the glycerine was drained first and Tilly's wash method employed. Experience has shown that even in a sealed bottle, a few days of settling allows for an absolutely clear product to form.

Any comments please.

LoganB
10-30-2006, 04:30 PM
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?

Tilly
10-30-2006, 09:32 PM
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.

Phild
10-31-2006, 04:28 AM
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?

Tilly
10-31-2006, 05:01 AM
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.

Phild
10-31-2006, 05:08 AM
Is there another way to process this oil i have 20gal heated as we speak?

Tilly
10-31-2006, 06:04 AM
Hello Phild

An Acid/Base method (http://biodiesel.infopop.cc/eve/forums?a=corfrm&cf=629605551) would probably work

Phild
10-31-2006, 06:20 AM
What is H2so4? And where do you get it?
(Thanks for the repleys Tilly)

Tilly
10-31-2006, 08:51 AM
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.

LoganB
11-01-2006, 12:45 AM
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.

Tilly
11-01-2006, 01:22 AM
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.

AndyW
11-14-2006, 11:53 AM
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?

domdom
12-07-2006, 08:21 AM
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. ?

Tilly
12-07-2006, 08:30 AM
Hello domdom, congratulations on your success

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

AndyW
12-07-2006, 11:45 PM
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.

Tilly
12-08-2006, 02:28 AM
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 (http://biodiesel.infopop.cc/eve/forums?a=tpc&f=9411061471&m=8281092351&r=8281092351#8281092351) (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.

AndyW
12-08-2006, 03:58 AM
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.


<span class="ev_code_RED">Tilly,</span>
<span class="ev_code_RED">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. </span>

<span class="ev_code_RED">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,,,,</span>

I recommend that the first and only test for completion required in most home situations is the WarnQvest Conversion Test (http://biodiesel.infopop.cc/eve/forums?a=tpc&f=9411061471&m=8281092351&r=8281092351#8281092351) (Pat Pend) which you refer to as the Methanol Test.

<span class="ev_code_RED">Yes, thanks, that is basically the test I am using.</span>

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.

<span class="ev_code_RED">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.</span>

<span class="ev_code_RED">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. </span>

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

<span class="ev_code_RED">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?</span>

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.

<span class="ev_code_RED">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.</span>

<span class="ev_code_RED">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. </span>

<span class="ev_code_RED">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.</span>

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

AndyW
12-08-2006, 04:24 AM
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.

AndyW
12-08-2006, 07:04 AM
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.

AndyW
12-08-2006, 07:14 AM
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.

Tilly
12-08-2006, 12:49 PM
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.

AndyW
12-08-2006, 03:49 PM
Hello Tilly,

Yes, your numbers sound right. This is why I went to huge efforts to make some coconut biodiesel. Out of a full litre, I ended up with only about 200 mils of the stuff. But it passes the water, methanol, boil AND the shake/bubble test with flying colours.

My basement shop is cool at about 60F and I can vouch for the fuel going cloudy real easy.

Most of the flying we do is in the summer anyway so this would not be a problem.

Coconut oil is expensive but so is ether and in any case it would be used to raise the cetane of a more common BioFuel. I'm anticipating that some sort of blend will give us that perfect fuel for all applications.

That run on B100 was actually on a pretty bad fuel but that I did manage to get it to run at all says volumes.

Winter has set in with a vengeance up here, Global Warming has been no help at all so all of this neat fuel I've got won't be tested for a few months, at least. All in fun but all of us may make a difference in the end. That's what we're here for and that's good.

Andy

Tilly
12-08-2006, 10:47 PM
Hello Andy

Are you using NaOH or KOH in your reaction?

In my experience clear Gels are soap caused when reacting with NaOH.
If you use NaOH in the reaction, When you evaporate the methanol out of biodiesel, soap will often settle out on top in a thin layer as you have described it.

If you are following the World Famous Dr Pepper Technique directions for making a litre of high conversion biodiesel from new oil (5g NaOH, 250ml methanol, react at 55deg C, an initial 40 good shakes followed by four more 5 second shakes over the hour) you should be making very high conversion biodiesel.
If you reprocess it using 4g NaOH/KOH and 100 ml methanol you will make lots of soap. Be aware that what is called the glycerine layer actually contains a LOT of methanol, probably 50% methanol in the first reaction when processing new oil.
The "Glycerine" layer of the second stage will likely be mostly methanol and soap. So the size of the methanol layer produced in the second stage is mostly dependant on how much methanol is used in the reaction and not an indication of how far the first stage reaction went.
There is a Hyperlink to the World Famous Dr Pepper Wash Technique (http://biodiesel.infopop.cc/6/ubb.x?a=tpc&s=447609751&f=719605551&m=741607061&r=741607061#741607061) (Pat Pend) in the World Famous Dr Pepper Technique (Pat Pend)
The fact that you are only achieving a yield of 200ml per litre of oil reacted suggests that you are making a lot of soap in the re-process. In my experience that is exactly what happens when you reprocess very high conversion biodiesel with 1g NaOH mixed into 50ml methanol.

All that is white is not soap.

The "Shake-um up" test has been shown over and over to be a meaningless test for quality. It is fine for showing the presence of soap.
Soap is at least as likely to cause an emulsion as an incomplete reaction. In my experience, if you use hard water for the test most biodiesel passes this test. If you use soft water most biodiesel fails this test.

I would have to do some tests before I put any faith in the shake and look for bubbles quality test.

AndyW
12-10-2006, 04:55 PM
Tilly,

Had a detailed reply and more input but,,,,

this is my third try at replying. I spent over an hour getting bumped off the reply page. don't know what's happening so I'll make this quick.

I'm going to go over the entire thread and do some more research. I have no doubt that temperature is my problem. We go down to 10C in the shop on occasion.

I'm of the mind that if we use more NaOH and let the mix settle overnight at warm temps we might have better results. Will test that premise.

Many, many thanks for your input and in fact, for starting this thread. We learn by reading, but mostly by doing.

AndyW
12-12-2006, 12:51 AM
Tilly,

As I understand it, the purpose of this thread was to offer a simple way that the newcomer to the making of Biodiesel can gain some insight and experience.

THAT you have accomplished in spades. And maybe this has been covered but we've done some experimenting and maybe we can shed some more light on problems some might have encountered.

First, I made up a batch of Sodium Methoxide, 250ml methanol and 5g lye. This was stirred and mixed for an hour to make sure that ALL of the lye was dissolved.

Then we added this mix to 1 litre of virgin, soy/canola oil, first heated to 70 degrees. Yes, a little hot but we lose some in the transfer.

This was given 100 violent shakes. The bottle was then set into a small tub of HOT water from the tap. Every fifteen minutes, 20 additional, vigorous shakes were applied six times.

Then the mix was allowed to settle in a special rig I made. This is pictured in the attachment.

This is a commercial product that is used to meter exact quantities of any sort of liquid. The cap fits any typical plastic gallon jug. It also comes with an adaptor that allows it to be secured to your common, 2 litre, soft drink bottle. It also fits a number of bottled water, bottles.

Included is a twist valve and a 20", clear, plastic tube with a stopper at the end. This was trimmed to three inches and an adaptor was applied to the open end carrying a short length of neoprene tubing. This is stoppered by a common paper clip.

AndyW
12-12-2006, 12:59 AM
The way this is meant to work is to isolate the "glycerin" that has settled from the good stuff above by using the valve. Once the sight glass is isolated, the bottle can then be set upright, the cap taken off and the fuel then transfered to a wash bottle.

Stoppering with a thumb while draining can work but perhaps some material that we don't want going back into the fuel is being left behind.

The next picture illustrates good conversion and settling of the "glycerin".

It doesn't look like a lot but this was allowed to settle for three hours. However, there IS a quantity of material contained in the valve and clear tubing.

AndyW
12-12-2006, 01:04 AM
The bulk of the settled material was drained out but stopped at where we could see some left, at the bottom of the clear tube. The level was marked as illustrated.

The main valve was left open and the device was tapped with a piece of dowel to dislodge any glycerine that my have been trapped therein. This was then allowed to sit for another three hours. No additonal glycerin settled out after that space of time.

AndyW
12-12-2006, 01:08 AM
HOWEVER, we noticed small globs of something, attached to the sloped sides of the bottle. What could they be? By tapping the sides of the bottle, we could dislodge these bits and they would promptly start sinking.

After ten minutes of tapping and observing, we found we had accumulated more glycerin. That is illustrated by the second mark.

AndyW
12-12-2006, 01:09 AM
These blobs are shown here.

AndyW
12-12-2006, 01:10 AM
And here.

AndyW
12-12-2006, 01:40 AM
OK, if those bits of glycerine were collecting on the sides, it would be reasonable to assume that there was still a quantity of glycerine in suspension.

So the rig was allowed to sit in the heated portion of the shop overnight. The heat was turned up and for 24 hours, our experiment was allowed to bask in 80 degree F heat.

The result, without any tapping to dislodge any material, can be seen below.

Entirely on its own, an extra 1.125 inches of material had settled. Adding the 3/8" inch that represents the first mark, we have 1.5" inches of additional glycerin settling out. That is, without any additional agitation to dislodge any of the globs that were now visible on the sides of the bottle.

Grabbing the bottle and twisting back and forth created a swirling of the mix and this action cleaned off most of the globs. They quickly settled and topped off the sight tube.

The clear tube's ID is 1/2" so my math tells me that overnight, we had an additional 24 ml of glycerine settling out, on its own, after 24 hours.

This rig is going to be allowed to sit for as long as it takes until no more glycerin makes its way to the sight tube.

Then we'll do the water and meth test.

Then we'll do the Dr Pepper wash and see what happens using the same rig.

AndyW
12-12-2006, 01:46 AM
I'm inclined to think that the cool conditions in my external shop created some of the early problems I encountered. Some nights it can get down to 40F.

So we'll see what we get, in the end.

Meanwhile, about washing. Here we have the results of a vigorous shake of good Biodiesel with distilled water. This is about a minute after a 20X shake.

AndyW
12-12-2006, 01:49 AM
And here's the result after 10 minutes. Crystal clear, colourless water with no, paper thin, white line of scum. Absolutely clean, Biodiesel. The bubbles you see on magnification are air bubbles. They rise and eventually, are totally dissipated.

Doing the meth test has the fuel go instantly into solution with another crystal clear, colourless result. In fact, a 50/50 mix was tried and still, the biodiesel goes into solution perfectly.

AndyW
12-12-2006, 02:10 AM
About the boil test. A recent batch of good fuel that passed the water and meth test did not come to a nice boil. Yes, this time I did it outside, on a hot plate, with a fire extinguisher handy.

Also, the shake and bubble test. Some batches of good fuel make lots of bubbles, others, not so much. Both the coconut and the olive fuel don't any make bubbles at all. Both have a notably lower viscosity than any of my other samples and both boil quite readily.

So again, it may simply be the type of oil used to make your fuel in any of this.

Once we have a repeatable procedure for making good fuel on the first pass, we'll be experimenting with using various types of oil.

AndyW
12-12-2006, 02:18 AM
About haziness and drying. A week if sitting in an open container would not allow the fuel to clarify. Yes, cool, basement shop. So I took a batch to the hot plate and heated. On this sample, I also did a boil test. Well, this good fuel, that passed the water and meth test, would NOT boil. Not even after it started to smoke.

What happened was that it turned a nice golden, more like orange colour. It didn't form any froth but I did get a clear, gel like material form.

That was filtered out as can be seen below. The filter is just a funnel with some fine, silk material as the filtering medium.

The gel was clear, but interestingly, the fuel lost its orange colour.

It's now clear and passes both the water and meth test.

AndyW
12-12-2006, 02:21 AM
But before boiling, this fuel that had been allowed to sit for a week, was transfered to another bottle and was filtered as a matter of course. The result was that the silk allowed the fuel to pass but water, in small globs, was held back. Surface tension action, I presume.

AndyW
12-12-2006, 02:29 AM
So to avoid the need for heating to clarify, maybe all we need to do is to allow the final wash to settle longer. A week? Two weeks?

With that in mind, we made up some adaptors for Dr. Pepper bottles as shown. These will attach to 6", clear vinyl tubing with a stopper on the end.

The tubing acts as a sight glass. As water collects, we drain and note the water level. When no more water accumulates, we assume a dry fuel. That will be tested.

Waiting till all the water comes out of suspension is much more energy efficient than having to heat it up.

AndyW
12-12-2006, 03:11 AM
And Finally. As you say, reprocessing as I've been doing it, appears to make soap out of a lot of perfectly good Biodiesel.

Some early batches pass the water test easily but don't pass the meth test.

What would you recommend to salvage this fuel?

AndyW
12-14-2006, 11:44 AM
OK, this is day three of our test of the Dr. Pepper method of making Biodiesel.

As related, we have followed the instructions to the letter. Plus, we have ensured that the temperature of the initial reaction was a tad higher than required. I'm assuming that this wouldn't hurt, could only help.

OK, after draining off ALL of the glycerin mix that had settled into the sight tube, we let the jug sit in the very warm shop overnight.

The result was that more material settled. AND, we have more of the globs of Glycerin stuck to the sides of the bottle. That is, the sloped sides. The vertical sides don't allow these to collect.

AndyW
12-14-2006, 11:48 AM
Without disturbing the material settled on to the sloping sides of the jug, we drained off the glycerin mix evident in the last picture.

By this time we had noted that three days of settling had allowed the upper part of the jug to clarify just a bit more than the lower section.

On the chance that there was a difference between the top of the mix and the bottom, we drew off a bit of the fuel from the bottom end.

Then we punched a very small hole an inch below the "water line" And squeezed some fuel from the top portion.

AndyW
12-14-2006, 11:51 AM
In some quarters, it is asserted that doing a water test on unwashed fuel gives an indicator of the quality of conversion.

So we did that test with both samples.

Here we see the samples one minute after shaking.

AndyW
12-14-2006, 11:52 AM
One hour later.

AndyW
12-14-2006, 11:53 AM
Three hours later.

AndyW
12-14-2006, 11:57 AM
So we appear to have incomplete conversion, according to some.

Next up is the methanol test. Remember, this is adding 10% fuel to 90% methanol.

My experience is that good fuel will be completely dissolve giving a crystal clear solution with no milkiness or haze.

In fact, good fuel will dissolve in a 50/50 mix of fuel to methanol,,, in my experience.

This is immediately after shaking.

AndyW
12-14-2006, 12:00 PM
However, 10 minutes later and we see oil settling out.

A half hour later and we see that about 25% of the test sample had settled out of solution.

We did not get a complete reaction.

AndyW
12-14-2006, 12:16 PM
So the question now is, WHY?

Did we use too much lye?

Not enough?

How about the quantity of the sodium methoxide?

A combination of the above?

And now what do we do? What might we do to determine where we went wrong?

There are two schools of thought as to how to re-process a bad batch.

The Dr. Pepper method calls for 50ml methanol with 1gm of lye.

The other, the JTF method, calls for 100ml of methanol and 3.5g of lye.

In this case, if we adjust for percentages, we see that the latter uses twice the lye, approximately.

And on top of that, the latter uses twice as much sodium methoxide.

Who's right?

If both called for the same amount of solution, that would be easy. You guys, ALL of you, never make it easy, do you? http://biodiesel.infopop.cc/groupee_common/emoticons/icon_mad.gif Me getting crabby again.

Sorry fellas but look at it from the point of view of the newbie. As far as I know, there's only one universe with one universal (get it?) set of physical/chemical laws. Yes, I know there's Newtonian physics and the other kind but lets' not go there.

For now, we have to assume that chemistry works one way. Add this to that at that or this temperature and EVERY SINGLE TIME YOU GET THE SAME RESULT.

No exceptions, no caveats. As someone said somewhere no magic involved. Wait, did he say only a little magic involved? Please,,, not very helpful.

So what to do? Here's what. split this batch exactly into half, halve the two sets of ingredients and give it a go.

THIS time, record the amount of "glycerin" produced and then conduct the water and meth test on both.

Fair? Right.

More later.

AndyW
12-25-2006, 11:33 AM
OK, finally, we have the test completed. Pictured are the ingredients according to two schools of thought fro reprocessing a bad batch.

AndyW
12-25-2006, 11:45 AM
And here we have the two batches settling out. The bottles on each end are other, ongoing, experiments.

AndyW
12-25-2006, 11:56 AM
Unfortunately, because my camera decided to kaff out on me in the middle of this, I can't give you any pics or specs on how much "glycerine" fell out from each batch. I didn't take notes, depended on the pics to record the data. Won't do that again.

However, there wasn't a great deal of difference between the two. I'm guessing that with the JTF formula, a lot of methanol remained in solution in the Biodiesel.

At any rate, each delivered a different result from the "water test" With the camera fixed, we can show this. On the left is JTF and the Tilly method is on the right.

Both look bad, each in their own way.

AndyW
12-25-2006, 12:01 PM
However, with some four, gentle washings, and a lot of filtering of white gunk, we got this.

AndyW
12-25-2006, 12:02 PM
And this.

AndyW
12-25-2006, 12:44 PM
Here we show the final wash for JTF.

AndyW
12-25-2006, 12:46 PM
And the final wash for the Tilly, reprocess formula.

AndyW
12-25-2006, 12:49 PM
Here's both, side by side, finished, perfect, biodiesel.

AndyW
12-25-2006, 12:52 PM
And, after sitting in opened bottom bottles to dry out for a day or so, we have crystal clear fuel.

AndyW
12-25-2006, 12:57 PM
Both batches pass the water test by 100% as well as the methanol test.

And both pass the bubble test with the Tilly batch making just one or two bubbles that pop immediately. Not bad, no complaints.

emiperformance
12-29-2006, 12:57 PM
Quick question,
I did a quick titration and got between 2-4 using NAOH. I did 3 1LTR test batches using 9, 10, and 11 grams of NAOH (these numbers include base of 7) all three batches seperated fine. the test batch with 11 looks the clearest. would I be safe using the test batch with 9 since it did seperate? I don't want to use more NAOH than I have to.

Thanks,
Danny

imported_pablovoncrunchnoble
03-21-2007, 05:13 AM
can't you try to react again with half cooked bio-d just to see if there are any left overs in solution-as the arguement goes on mixing the more mix the better the results up to the prescribed time. What is going on with the 2.5 minute reaction that greenstar is using and who is using ultrasound to break the glycerin out of bond.

dodgechick98
03-22-2007, 05:51 PM
In my case, the lye never fully dissolves in the methanol. I use a drill to mix and even after at least an hour, there is still lye undissolved at the bottom of the tank. Any ideas on how to make the lye dissolve?

johnwontok
03-27-2007, 01:03 AM
hi all:
gotta question. the titration i did on my used wvo was high. it took 8mm of 1% NAOH to get a color change on 1ml of oil in 10ml of alcohol. so...with a base of 5g/liter required to convert unused oil do I add 8g/liter (titration results) additional NaOH for the reaction to take place properly?????

john

Joe_M
03-27-2007, 12:03 PM
No, you go look for better oil. And DON"T EAT at that place! http://biodiesel.infopop.cc/groupee_common/emoticons/icon_eek.gif
But seriously, how many times did you do the titration? That's about 15 grams per liter of oil, seriously nasty stuff or something wrong. Could be dissolved acids like vinegar in the oil. Wash the oil, dry it, and try again. If it is still that high, go somewhere else. HTH http://biodiesel.infopop.cc/groupee_common/emoticons/icon_smile.gif

imported_totalcheapskate
05-23-2007, 12:36 PM
have just brought 4.2 diesel landcruiser 1992, made two batches of dr pepper method, both with 1lt of wvo, first with 250ml methylated spirits and 7g caustic soda crystals ( mixed at room temp in june uk, turned to a jelly like substance with in few hours but no 10 min reaction, slowly producing liquid that is clearer and runnyer than oringinal oil but this is after 3 weeks and still only produced about 300ml and still jelly based in bottle, second used 250ml methylated spirits and 10g of caustic soda as before , oh my god i've just invented brown mayonnaise!!!! which hasn't changed in two weeks, also got a price from catering suppliers of approx £15 per 20 litre drum of fresh veg oil, yet people are quoting any where from 25 to 42 pence per litre ( not a cold fusion scientist so my maths may be a little out but to me that doesn't work ), and as for tritration, easy for people who say their already doing it, but not even a four year old can understand the explanation on here, i've tried and my daughter kepps asking for the cbeebies web site, acn any one help with a recipe that should work with wvo with out tritration, or a tritration recipe that works, before bankrupcy sets in from fueling tne landcruiser,

many thanks

Tilly
05-23-2007, 01:13 PM
Hello totalcheapskate, welcome to the colourful world of biodiesel.

Methylated spirits is typically about 95% ethanol and 5% water in ลึก ประเทศ*ินเดีย . This is EXTREMELY unlikely to make biodiesel.
You need to obtain some 98- 100% methanol for the reaction.

On the positive side, your failed batches will not count towards your annual allowance of 53.459 litres of Royalty free biodiesel http://biodiesel.infopop.cc/groupee_common/emoticons/icon_wink.gif

imported_totalcheapskate
05-24-2007, 09:31 AM
cheers tilly, thnaks for the direction, i have tried to locate methanol from two local chemical traders, one frefused to sell me any as it would be private sale and they only sell to companies (told they have a responsability of care for whom they sell to so as they were confused by the whole bio diesel explanation they refused, second company had loads of people buy methanol off them for bio-diesel but no one return a second time , they were charging silly price thet made the whole process more expensive than fossil fuel. any advice to were to purchase and are they different qualities/ ie gold/silver/bronze quality etc, also are you based in uk?

cheers

TCS

imported_totalcheapskate
05-24-2007, 09:33 AM
quick thought, could i boil methylated spirits to remove water as can be done with oil? may be a stupid question but if you don't know the answer it isn't a stupid question!

cheers

Tilly
05-24-2007, 09:37 AM
Hello totalcheapskate

I understand that methanol is hard to get in the UK. If you do a search on this forum I believe there are a few UK members that do sell methanol.
Another thought is that Model plane fuel is made from methanol+ other things. Here in ลึก ประเทศ*ินเดีย it is common for Model clubs to have a drum of methanol to sell to members. You may find something similar in the UK.

Tilly
05-24-2007, 09:39 AM
Hello totalcheapskate

No, 95% is about the best you will get out of a still without adding another chemical.
In any case you will end up with ethanol which is not particurlarly reliabel in the biodiesel reaction.Originally posted by totalcheapskate:
quick thought, could i boil methylated spirits to remove water as can be done with oil? may be a stupid question but if you don't know the answer it isn't a stupid question!

cheers

James2
05-27-2007, 08:11 PM
Hi Tilly,

Something funny happened. A week or so ago I made my first test batch using the Dr Pepper method. Worked great! I let it sit for a while and it became very clear. Then, yesterday I bumped it and noticed little bubble-looking things that were floating DOWN toward the glycerin. Then today, the biodiesel seems slightly cloudy. Not super cloudy, just not super clear like it was before I bumped it. Note that it didn't fall over, just moved a little bit. I didn't even swirl it.

What happened?

Tilly
05-27-2007, 08:38 PM
Hello James

Did the biodiesel get cold? If it got cold it could be high melting temperature esters solidifying and settling the bottom of the bottle kind of like it is snowing.
This can form a white layer on the bottom.
If you move the bottle this layer will often look like smoke moving .

James2
05-29-2007, 04:46 AM
Hi Tilly,

I don't think it would have gotten colder than about 68F. It didn't seem like snow, more like bubbles floating down. Anyway, now it's clear again. Funny.

James2
05-29-2007, 02:32 PM
Hi Tilly,

Update - I just checked the temperature outside and it's 66F. I think this is about the coldest it gets during the night. And, it's cloudy (the biodiesel, that is). Is it temperature-related?

mp11
07-07-2007, 08:11 PM
Hello all. I just did my first test batch using the Dr Pepper methode. I used 250 ml methanol, 4g NaOH, and 1 liter of new oil. After shaking for about 10 seconds, it started separation about 5 minutes after. After 2 days, it has cleared some, but not as much as I expected. But then maybe this is all it will clear? I moved it around a bit a while ago, and I noticed some gel formed on top of the glycerine. There is also a thin film of what may be soap on top of the biodiesel.

So my question is, what should I do about it? Should I remove the biodiesel and do the Dr Pepper bottle wash? Thanks in advance. Here is a pic of my first test batch.

Tilly
07-08-2007, 08:37 AM
Hello mp11, welcome to the forum and congratulations on your first successful batch of biodiesel!
It looks perfect.
4g NaOH is a bit short, but yes, go ahead and do the wash.
And remember, Gently, gently, gently is the prime directive.

mp11
07-11-2007, 12:44 AM
And...just to follow up. Here's a pic of the sample after washing and drying. Doesnt look too bad actually. http://biodiesel.infopop.cc/groupee_common/emoticons/icon_smile.gif

On a side note: I did a second 1 liter test batch using a blender. The blender actually churned much too fast and I made a nice batch of soap basically. Kept trying to wash it, but wound up with more and more soap and less and less biodiesel in the dr pepper bottle. So I gave up on that.

BDMike
09-06-2007, 05:08 AM
Hi Tilly, I keep reading that CARTRIDGE RESPIRATORS DO NOT WORK WITH METHANOL in several of your posts. I was wondering which type you recommend and where do you get them. Thanks

Tilly
09-06-2007, 06:53 AM
Hello BDMike

The only respirators that are safe to use with methanol are the Supplied Air variety

JerseyWreckDiver
09-23-2007, 08:30 PM
Hi,

Well I finally went shopping for soda bottles and new vegatable oil to try my first refining of biodiesel. I used the addended method of shaking 4 times over the course of an hour. and after 24 hours I have a bottle that looks like mp11's first picture, clear glycerin on the bottom and not so clear bio on the top. For whatever reason, like mp11 I was expecting something more clear on the top... Should I wait another day or is it good to wash?

Also, I'm easily confused, I separate the bio & glycerin first? Any prefered method for this? Just pour off the bio? Won't the glycerin try to come to the bottom as I pour...

I've started reading into the almost 400 posts on this thread and someone mentioned something about the glycerin solidifying...is this something I should expect? Want?

In other forums I've asked about disposal of the by-product and people have suggested making soap and such, but I've read here that a fair percent of the methanol is in the by-product... Isn't this highly toxic?

Thanks for the help and Tilly thanks for putting this on the net to make getting started easy for the rest of us.

Tilly
09-24-2007, 08:20 AM
Hello Kylie, congratulations on your first successful batch of biodiesel!

What you describe is as it should be.
It is ready to wash.
Yes, seperate the glycerine and biodiesel first.
If you used NaOH/Caustic soda, the glycerine will likely eventually solidify, but as you have used new Veggie oil and plenty of methanol it will take some time.
Yes, the "glycerine" straight from the reaction is toxic.
You are welcome.

imported_psi3000
09-27-2007, 09:33 PM
Hey guys,
I have a quick question. I tried the Dr.Pepper way two times. The first time I used Zep 10 min drain opener. And when I did it it didn't turn brown at all. Today I saw a lower darker color layer on the bottom, not much at all. So I went and bought the Robeic crystal drain opener displayed on the site. This didn't "change color from a "Chocolate milk to a rich, darker brown" in the beginning or in the next 10 mins like your site says. I am using the cheap walmart brand vegetable oil and the yellow Heet. Using 4g of NaHO and 250ml of the Heet. I don't know if this is normal to miss the dark brown stage . Am I doing something wrong. Is there a variable I'm not seeing.
thanks
rich

Tilly
09-27-2007, 10:09 PM
Hello psi3000, welcome to the forum

It sounds like you are using new veggie oil.
If you look at the instructions it says,
"If you used New Oil, the colour change is not nearly as great and you may have problems seeing much of a colour change at all.
If you reacted New Oil the glycerine layer on the bottom will not be much darker than the oil you started with and the biodiesel will usually be very light in colour.
The biodiesel will be very cloudy, and it will take a day or two more for it to clear."

Check to see if you can see two layers in the bottle. The bottom layer will usually be slightly darker and clearer than the top biodiesel layer.

imported_psi3000
10-02-2007, 04:53 AM
OK, I see that now. And yes, there is the darker layer on the bottom of both test batches. However, I washed one of the batches three days ago, like described on the site, and the one I did'nt wash is way more clearer than the one I did wash and it has been three days. I did these test runs because my friend has 55gal of filtered twice veg oil that he used for his SVO VW he used to own. So I am going to use two 55gal drums welded together for my primary tank, and I just wanted to make sure I had the theory and idea/what to watch out for, before I ran a 55 gal batch through the process. So I think my final questions are: Is this normal or do I just have to wait longer? Do you have to wash clean veg oil?

Tilly
10-03-2007, 05:52 AM
Hello psi3000

Washed biodiesel always starts off cloudy.
The spead at which it drys/clears depends on many things, such as temp, humidity, in the sun or in the shade, is the top open or closed etc.

What do you mean "Do you have to wash clean veg oil?"
Most people do not wash the vegie oil.
Most people either water wash or dry wash or magnasol wash the biodiesel.

imported_psi3000
10-03-2007, 01:52 PM
I mean do you have to wash the biodiesel if you made it from clean, store bought vegetable oil?

Andrew M
10-03-2007, 04:33 PM
Too wash or not to wash is a (slightly) open question.

Some have used unwashed fuel with no apparent side effects.

Most here agree that it is best to remove the methanol and soaps.

The washing is not related to the WVO being dirty, but to the removal of the remaining contaminants from the BD reaction. If you think you should wash BD from WVO, then you'd also want to wash BD from virgin oil.

HTH.

imported_psi3000
10-04-2007, 04:59 AM
thanks soo much for the info. I checked my biodiesel made from store bought veg oil and it was much clearer today. I am going to make my tank this weekend and start a batch. You guys rock!

gquatro74
10-26-2007, 07:00 PM
ok so i tried and failed. i had a few problems
so maybe you guys can help me out.
1. the lye i got said sodium hydroxide.
however the composition of the drain cleaner
had crystals, white balls and blue balls.
im assuming oonly the crystals are the hydroxide?
2. i think i may have burned the oil, also oil was used and unstrained. are these problems?
3.i used methyl alcohol gas line antifreeze. is this the same as methanol?
4.the oil was the warm but i didnt have a gauge to get 60degrees when i mixed it with the methoxide.

The methoxide was blue in color. my attempt at biodiesel made a small layer at the top and bottom with a big one in the middle. all are dark browns.

\thanx in advance

Bunk
10-28-2007, 12:23 PM
Originally posted by gquatro74:
ok so i tried and failed. i had a few problems
so maybe you guys can help me out.
1. the lye i got said sodium hydroxide.
however the composition of the drain cleaner
had crystals, white balls and blue balls.
im assuming oonly the crystals are the hydroxide?
2. i think i may have burned the oil, also oil was used and unstrained. are these problems?
3.i used methyl alcohol gas line antifreeze. is this the same as methanol?
4.the oil was the warm but i didnt have a gauge to get 60degrees when i mixed it with the methoxide.

The methoxide was blue in color. my attempt at biodiesel made a small layer at the top and bottom with a big one in the middle. all are dark browns.

\thanx in advance

Hi gquatro74. Welcome to the forum.

1. Sodium hydroxide is white in color. It sounds like you tried Draino. Draino doesn't work for biodiesel. Roebic brand "Heavy Duty Crystal" drain cleaner is sodium hydroxide and will work. I don't think any of the liquid drain cleaners will work.

2. Titration (http://biodiesel.infopop.cc/eve/forums/a/tpc/f/719605551/m/9541092001) is the best way to check how "burned" your oil is. If your oil has any water in it that could cause the batch to fail. Food bits tend to hold water easier than oil so it's a good idea to strain it first. Read CBT: Testing Oil for Water. (http://www.biodieselcommunity.org/testingoilforwater/)

3. I'm not sure what kind of gas line antifreeze you tried but Heet gas line antifreeze in the yellow bottle is methanol and will work fine for making biodiesel.

4. I don't use a thermometer when doing test batches either. Floating the capped bottle of oil in a bucket of hot tap water seems to get it warm enough. Once you add the sodium hydroxide dissolved in methanol, seal it up again, give it the recommended number of shakes, and drop it back in the hot water bath.

I'm not sure what you made in your first test batch but don't consider it a failure. It was just a stepping stone to success.

Ken

brownhousechris
11-14-2007, 02:31 PM
Hi all,
I've made my first Dr Pepper method batch of biodiesel, using lab-grade methanol and sodium hydroxide, and filtered/dewatered WVO. Everything went beautifully, until I came to the 5th wash. All the washes were going great, but I really shook the 5th wash hard, and after that I have been left with what looks like Tang: orange colored and very cloudy. I've waited two days, and just did a 6th, gentler wash. So, I'm not sure what to do now. Did I ruin the batch, or does it just need lots more time? Would it help to leave it uncapped? Should I give up? Any advice would be greatly appreciated.

Bunk
11-14-2007, 08:46 PM
Welcome to the forum and congratulations on your first batch!

I'd leave it un-capped in direct sunlight for a day or two and see what happens. A window-sill would be ideal unless you have small children or pets. Put something under the container so it doesn't get on the finish of whatever surface you decide to put it on. Biodiesel is known to be a good solvent.

Ken

10.90streetcar
11-19-2007, 07:25 PM
Just made my first test batch. All looks good but I lost a lot of oil/bio diesel in the process. Is this normal?

http://i134.photobucket.com/albums/q120/1090streetcar/bio1.jpg
http://i134.photobucket.com/albums/q120/1090streetcar/biowash.jpg
http://i134.photobucket.com/albums/q120/1090streetcar/biodone.jpg

brownhousechris
11-20-2007, 05:14 PM
Thanks, I'll give that a try. I've left it on the windowsill for a couple days, and it does seem to be clearing. If it does clear, should I wash it some more?

Tilly
11-22-2007, 04:33 AM
Hello Streetcar

It looks good, I would not wash it again.
As you get some practice you will not lose much product.

brownhousechris
11-27-2007, 07:22 PM
Great, it cleared up a lot! It now looks much more like other pictures I have seen. So, now what? Should I just take the little water off the bottom and use it, or should I wash it some more, since it formed such an emulsion? When would it be safe to pour into the tank?

bmor
12-05-2007, 09:17 PM
Well I (as a newbie) also just made my first 1L test batch using the famous Dr Pepper method. I was planning on using some used oil but my contact had already cleaned the fryers so he just gave me a litre of fresh Canola. After 24 hrs I seem to have gotten good seperation, however the product seems cloudy. I did it in my garage and the room temperature could be causing this. I'll check it again tonight (48 hrs since reaction.) Next I guess it's time to do a wash. One question; How do I remove the good BD from the glycerin? If I go to pour it it seems like the glycerin will come out as well. It doesn't seem like it will stay on the bottom of my container.

SamSla
12-07-2007, 07:08 PM
I'm a newbe and color blind so I don't think titration will work for me. Does anyone here use a pH meter instead of titration? If so, how do you do it?

Tilly
12-08-2007, 09:29 AM
Hello SamSla, welcome to the forum

Perform the titration as per the World Famous Chopstick Titration Technique (http://biodiesel.infopop.cc/groupee/forums/a/tpc/f/719605551/m/9541092001) (Pat Pend) and use the pH meter instead of an indicator. A pH of 8.6 is the magic number.

SamSla
12-08-2007, 12:30 PM
Thanks Tilly. That's just what I needed to know.

buckied
12-10-2007, 01:40 PM
hey, did any of yall see the article in Diesel Tech Magazine on Tilly's Dr. Pepper Technique...good write up!

GrahamLaming
12-10-2007, 02:12 PM
Hi SamSla

You should be fine with just the visual change - even if color-blind, the change is clear and obvious.

Take a look at this page for a comparison...
Indicator Comparison (http://www.graham-laming.com/bd/titration_indicator_comparison.htm)

Biodiesel Systems
12-13-2007, 05:12 AM
Can someone please explain the difference between esterification and transesterification?

Graydon Blair
12-13-2007, 05:20 AM
Esterification is where you use an acid to modify the free fatty acid chains to allow methanol to bond to them to form Biodiesel.

Typically, Sulfuric Acid is used.

Transesterification is where you use a base as a catalyst to break fatty acid chains away from a glycerol molecule and then allow methanol to attach to them.

Typically, Sodium Hydroxide (NaOH) or Potassium Hydroxide (KOH) is the base used.

Esterification is commonly called the "Acid" method.

Transesterification is commonly called the "Base" method.

Esterification reactions are much much slower than Transesterification reactions.

If oil titrates really high, an "Acid" method can be used to "lower" the titration down because it modifies the free fatty acid chains into Biodiesel.

Most people will do both an Acid and a Base reaction together if they make Biodiesel.

This is because the Esterification process will allow for higher yields of Biodiesel vs. just using a normal Base method if the oil Titrates really high.

If a normal "Base" (Transesterification) process is used, the majority of the free-fatty acids get converted into Soap instead of into Biodiesel.

-Graydon

daw
12-13-2007, 05:26 AM
WOW!!! I knew there was a reason I got on here tonight. I've learned something new. I had no idea one was the acid process and the other one was the base process.

I've always just called "it" transestherfication (or is it transestherification?)

Thanks, Graydon!!!

Andrew M
12-13-2007, 05:38 AM
Yes, acid stage is esterification, since FFA is not an ester. Base is transesterification, (changing one ester to another) since triglyceride is an ester, and so is FAME.

Graydon Blair
12-13-2007, 07:10 AM
Originally posted by daw:
WOW!!! I knew there was a reason I got on here tonight. I've learned something new. I had no idea one was the acid process and the other one was the base process.

I've always just called "it" transestherfication (or is it transestherification?)

Thanks, Graydon!!!

And now you know the two biggest words in Biodiesel!

I've met a lot of seasoned Biodiesel home-brewers out there that have no clue what it actually means. Plus, it's just a cool word. "Transesterification."

-Graydon

Biodiesel Systems
12-13-2007, 02:16 PM
thank you Graydon

olaf455
01-02-2008, 03:48 AM
First success... Yea... Just made a quality batch using the "World Famous Dr Pepper Technique (Pat Pend)"... Don't worry, the royalty check is in the mail... What can I say the process works, and with 12 year old "new" canola oil...
I did get a few globs of what looks like soap(white solidish waxy looking things) formed in the individual "feet" of the dr. pepper bottle... Bio D is quite good looking otherwise... Gunna wash it tomorrow... How long should I wait for settling to occur before
pouring off the bio d?
This forum is a blessing, as I unfortunately discovered the jtf website first... Ikky...

Thank you in advance for any help.


The smoke don't mean it's broke...

Legal Eagle
01-02-2008, 12:08 PM
This forum is a blessing, as I unfortunately discovered the jtf website first... Ikky...
Yes it is."Ikky" has also been refered to as The Cult due to the way it is run. Welcome to the forum, and congrats on your entering the wonderful world of biodiesel.
Do yourself a favour and read The Colaborative Biodiesel Tutorial (linked in my sig line)

olaf455
01-03-2008, 03:16 AM
Well I washed the bio d today and after about 6 washes the stuff actually looks respectable... Tomorrow I will heat it to remove excess water and see what we get...
I have been studying the water free method and will incorporate this on an upcoming test batch...

Next up is to find some wvo and learn to titrate. Should be great fun. Thanks all...

TheGreenMan07\'
01-07-2008, 11:13 PM
Hi all. I've been running wvo in my cummins for about a year and a half and am now thinking about making some bd for long term storage and everyday use. I have performed the dr pepper on a new litre of oil. everything looks good so far. What does the bd smell like? Mine kinda smells like butter, like I would not mind it on my toast. I looks like the pics but I thought it would smell different. I did five washes but I dont think I'll wash during production. Any comments would be great!!!

olaf455
01-08-2008, 12:10 PM
Depends on what you made the bd out of. Mine smells quite similar to the canola oil it's made of.

As far as washing, check out Gram Laming's 1 day process / airwashing.

chris szm
01-16-2008, 10:01 PM
hey tilly ,,you still alive i see..you dont probably remember me from a few years ago..??i had a go at your dr peper technique for using drink bottles http://biodiesel.infopop.cc/groupee_common/emoticons/icon_biggrin.gif...
i havent been on for ages i got sick of all the armchair chemists going on and on ..
im still making bd by the 160 lt batch and i dont wash..im on my third car now with lots of km on 100% bd ..i dont have a problem with it at all just keep your filter changed regular..
anyway good to see you still hear ..is biocruiser still on??
cheers chris

Tilly
01-16-2008, 10:18 PM
Hello chris

Yes, I remember you.
It has indeed been a long time.

Biocruiser still posts from time to time, but not often.
I am glad to hear that your cars never learned they were supposed to fall apart from using unwashed biodiesel.

Amy Wu
02-03-2008, 04:35 PM
How can you possibly put 140 degree F oil into a plastic soda bottle?
The oil would immediately change the shape of the bottle. Also, even with gloves, how could you possibly shake the bottle when it's that hot?
Thanks

Amy Wu
02-03-2008, 04:39 PM
Also, how do you remove the biofuel from the glycerin once it's settled to the bottom?
and the NaOH that I have is dissolved in water, I think its 50% NaOH, 50% water, could I use that instead of a drain cleaner and how much would I use?

Tilly
02-07-2008, 01:53 PM
Hello Amy, welcome to the forum

I am sory I missed your post.
I have performed the reaction with oil at a temperature of 62deg C (143deg F) as I poured it into the bottle with no damage to the bottle.
However, I can see your concern and I will change my recomendation from 60deg C or less for WVO to 55deg C or less which is in line with my recommendation for new Vegie oil.

I just pour the biodiesel carefully out of the bottle and may leave a slight bit of biodiesel with the glycerine.

Yes, you can use aqueous NaOH, but at this point I do recommend the anhydrous type.

crash_harder
02-27-2008, 12:06 AM
hello all, like a lot of ppl i have just started doing this. i love it!! i do have a question though. in tilly's way it calls for the "yellow" bottle of heet aka "methyl alcohol". i made a batch last night, didn't have a good scale though so i got a scale today after work and made another batch with the "yellow" bottle. i also grabbed a "red" bottle of heet aka "isopropyl alcohol". the lye just will not disolve in the "red" bottle... i am not even close to being a chemist... my question is, is the red and yellow bottles the same when we use it for BD?? or should i never buy the red bottle again...

thank you and AWSOME FORUM

crash

Bveggiecruiser
02-27-2008, 05:04 AM
Hey there Tilly yep still sticking my nose in from time to time

Chris szm yet member you to can I help u ?


BC

Tilly
02-27-2008, 06:09 AM
Hello crash, welcome to the forum!
The red and yellow bottle are not the same.
Use the isopropanol in the red bottle to do the World Famous Chopstick Titration Technique (http://biodiesel.infopop.cc/groupee/forums/a/tpc/f/719605551/m/9541092001) (Pat Pend)
Use the methanol to do the reaction.

crash_harder
02-27-2008, 04:47 PM
thank you!!!

i must say, this bio diesel thing is the best thing since sliced bread!!

Knotwild
03-11-2008, 07:31 PM
I made my first liter kitchen batch Saturday and have a few of questions. My titration called for 5.2gm of NaOH, so I used Roebic drain cleaner as 100% NaOH and 20% methanol (yellow HEET bottle). I also heated the peanut oil to 130F and used the 4 shakes in an hour method to mix it. I was using penut oil that had been heated to remove the water and had only cooked one turkey at Christmas. I have not done the 3/27 test yet.



1: I tried to titrate my Isopropl alchohol before doing an oil titration, but I never could get the Heet (red bottle) to turn red. Is this a common problem and should I even worry about it?

2: I noticed some sedimentation that can best be described as snowflakes falling to the bottom of my flask.
It was most evident after washing, so I attributed it to remaining water causing formation of soap. It
continued to form in small amounts for 48 hours after the reaction. I drained it off each time I saw it.
It stopped settling after I strained it through a coffe filter twice. Is that a problem and was it soap?

3: After filtering, the product can best be described as apple juice in color. I took it outside this
this morning and exposed it to 42 degree temps whereupon it turned to solid in about 10 minutes. Is
this normal and helped by adding anti-gel agents?
4: What range should my final ph be in?

Thank you in advance for your help.

Bunk
03-13-2008, 03:12 AM
Originally posted by Knotwild:
I made my first liter kitchen batch Saturday and have a few of questions. My titration called for 5.2gm of NaOH, so I used Roebic drain cleaner as 100% NaOH and 20% methanol (yellow HEET bottle). I also heated the peanut oil to 130F and used the 4 shakes in an hour method to mix it. I was using penut oil that had been heated to remove the water and had only cooked one turkey at Christmas. I have not done the 3/27 test yet.
Congratulations on your first batch.

1: I tried to titrate my Isopropl alchohol before doing an oil titration, but I never could get the Heet (red bottle) to turn red. Is this a common problem and should I even worry about it?
I don't think that's common. It should go red if you use turmeric. If you use phenolphthalein it's more of a purplish color. When doing titrations I push for the same color change that I get when blanking the isopropyl.

2: I noticed some sedimentation that can best be described as snowflakes falling to the bottom of my flask.
It was most evident after washing, so I attributed it to remaining water causing formation of soap. It
continued to form in small amounts for 48 hours after the reaction. I drained it off each time I saw it.
It stopped settling after I strained it through a coffe filter twice. Is that a problem and was it soap?
For some reason peanut oil makes snowflakes sometimes. I don't know why it happens but it happened to me before.

3: After filtering, the product can best be described as apple juice in color. I took it outside this
this morning and exposed it to 42 degree temps whereupon it turned to solid in about 10 minutes. Is
this normal and helped by adding anti-gel agents?
Different kinds of oil will make biodiesel with different gel points. I use soybean oil and it starts to cloud at about 35°F and is gelled at about 30°F. Mixing diesel fuel or kerosene in it can lower the gel point some. I have never tried anti-gel agents.

4: What range should my final ph be in?
Final pH of what?

Ken

rockfrawg
03-13-2008, 09:33 PM
howdy all!

i think it hit me about the same time it hit quite a few other people...when I saw $3.99/gal for diesel i decided it was time...

Just finished making my 1st Dr. Pepper batch. Made 3L using store bought vegetable oil, 2 bottles of HEET (710mL), and 1/2 tbsp of 100% lye...oh...and i'm using the 4 shake method. Gonna get a scale tomorrow to weigh the NaOH so that like someone said, I can keep it consistent. A 750mL empty Absolut vodka bottle worked nice for mixing up the methoxide...just the right size for the batch I made (at least I hope anyway). Let me know if it sounds like I mixed anything wrong.

Any tips for getting the BD out once the glycerin settles? also...where might I find some info about drying...havent made it that far in the research yet, hope to be able to wash tomorrow. Thx for being here y'all, I hope this works out so I can completely do away with the necessity for fossil diesel...$4/gal...rediculous...

Andrew M
03-13-2008, 09:52 PM
Wellcome, rockfrawg,

There is a huge wealth of info right here if are willing to play with the search feature. Also, check out the colaborative biodiesel tutorial, in my sig. line. The info there is a little easier to navigate, but summarized.

To separate, a funnel with a valve works well for small batches. Just drain the byproduct layer off.

Good luck, and have fun!

rockfrawg
03-15-2008, 01:59 AM
alrighty...probably no big deal but just wanted to ask...so, all was going well until I got to what I thought might be the final shake in the wash process. I had about 3L of BD before that step (i'm using a 3L Ozarka bottle). After that wash, when draining the water it was extra soapy compared to the prior washes. I lost about 20% of my final product and since letting it settle a white layer has formed on the bottom of the jug. Its not as bad as what it might look, the center of the jug is recessed upwards so it make the jug look like it holds quite a bit more than it actually does, and at the same time makes the stuff thats settling to the bottom look like about 30% more volume that it actually is. I'm just curious what this is. It should be fairly easy to drain off but it seems that every time I drain stuff I lose part of my BD.

TIA for any input

PS. I've attached a pic of my "tools" just for your enjoyment, sorry for the size, my file hosting program no longer resizes them automatically for me.

www.texasoffroad.net/albums/lonestar/album309/DSC05310.jpg (http://www.texasoffroad.net/albums/lonestar/album309/DSC05310.jpg)
www.texasoffroad.net/albums/lonestar/album309/DSC05311.jpg (http://www.texasoffroad.net/albums/lonestar/album309/DSC05311.jpg) www.texasoffroad.net/albums/lonestar/album309/DSC05315.jpg (http://www.texasoffroad.net/albums/lonestar/album309/DSC05315.jpg)

TRUUBLE
03-19-2008, 12:39 AM
WOOO HOOOO!!!

It worked!!

The reaction occurred just as described and it's clarifying as we speak.

I always have drums of methanol around, because I run it in my race car. I have a Chinese restaurant lined up that will give me their oil. Now, all I need to do is build the reactor!!

garym364
03-26-2008, 10:19 PM
we just tried our first batch in soda bottle. It stays dark and has good settling on the bottom. It has been 1 day since it was mixed. Should we wait til the bottom gels bofore washing or seperate while still liquid.
Thanks

Bunk
03-26-2008, 11:11 PM
Congratulations on your first batch. You can separate it while still liquid. Be careful not to let any of the byproduct get in with the wash. It may cause an emulsion. (http://www.biodieselcommunity.org/breakingemulsions/)

Ken

Timothy
03-29-2008, 01:26 AM
Hi everyone. I've also finally got around to trying the Dr. Pepper. Followed the steps as closely as possible. I noticed though, that something was wrong when I opened the bottle of draino. It had little metal flakes in it. The caution on the bottle listed Sodium Hydroxide so I figured that it was the right stuff. I went ahead thinking that I could just strain out the metal flakes when I remeasured the 250 mils. I really felt like something was wrong when the 3rd and 4th hour of fairly vigorous mixing occured. It was supposed to take 10 minutes?
Anyhow, I used waste oil that I've had for about 6 months and put through 2 layers of cheesecloth-looked pretty clean and couldn't get any water poping when I heated it up.
When I added the Methoxide and shook it up for 10 seconds it took on the cloudy light chocolate milk appearance but then almost immediately settled with a layer (about an inch) of clear-oil coloured liquid and about 6 inches of the same colour-only cloudy. I measured the lye using a teaspoon, the Methanol I used was Methyl Hydrate-(same thing?). Something doesn't quite fit with the description. Any thoughts?

Bunk
03-29-2008, 02:58 AM
I tried Draino once. It didn't work for me either. 100% Sodium Hydroxide can be found as "Red Devil Lye" drain cleaner in some hardware stores. The best method to measure the sodium hydroxide is by weight. You can make a balance scale from ordinary household items that will work well enough for 1 liter test batches. See the Dixie Cup Scale (http://www.biodieselcommunity.org/dixiecupscale/) page at the CBT. They suggest using measured amounts of water for the balance weight but US pennies minted after 1983 weigh 2.5 grams each. Five grams sodium hydroxide per liter of oil is a very common standard amount for new vegetable oil. That would be the same amount as what two pennies weigh.

Wikipedia (http://en.wikipedia.org/wiki/Methanol) lists methyl hydrate in the "other names" section of the methanol page. Purity of the methanol is important. If you doubt the purity of your methanol, HEET gas line anti-freeze in the yellow bottle is pure methanol. Be sure to get the yellow bottle. Iso-HEET in the red bottle won't work.

Ken

Timothy
03-29-2008, 02:22 PM
Thanks Ken,

The Methyl hydrate lists 99.9-good enough? I think that I'll try finding better lye.
Now -what to do with that nasty Draino. I guess I'll wait for Hazardous Waste day to dispose of it.

Tim

Bunk
03-29-2008, 02:39 PM
The Methyl hydrate lists 99.9-good enough? I think that I'll try finding better lye. Now -what to do with that nasty Draino.

99.9 should work very well.

I think I'd dispose of the Draino by using it to clean my drain pipes. Be sure to follow the directions on the can.

Ken

Superorb
03-29-2008, 11:45 PM
Hi all. I tried making a test batch, and I don't know if it worked correctly. I spilled a small portion of the methoxide mix (mason jars don't pour well) and after an hour there's only about a 1/4" of clear fluid at the top with the cloudy/milky portion below that. Also, the bottle is starting to deform, can I loosen the cap to let some air in the right the bottle again? Last one, after the glycerine settles to the bottom, how do I separate it out of the 2L bottle? Thanks.

Tilly
03-31-2008, 01:43 AM
Hello Superorb, welcome to the forum

Did you use new oil or WVO?
Is there a thin layer forming on the bottom?
The thin layer on top is likely to be the meniscus.
Yes, you cal loosen the cap and allow air inside

Superorb
03-31-2008, 01:50 AM
Originally posted by Tilly:
Hello Superorb, welcome to the forum

Did you use new oil or WVO?
Is there a thin layer forming on the bottom?
The thin layer on top is likely to be the meniscus.
Yes, you cal loosen the cap and allow air inside
I used new oil. Looks like this:

http://i168.photobucket.com/albums/u177/superorb/Misc/_MG_0789.jpg

Tilly
03-31-2008, 01:56 AM
Hello superorb, congratulations on your first successful batch of biodiesel!

It looks perfect for new oil.
Because you used new oil, the glycerine layer on the bottom is not particurlarly dark.
The "thin layer" on top is actually the meniscus (http://en.wikipedia.org/wiki/Meniscus) of the biodiesel.

Superorb
03-31-2008, 02:11 AM
Ok. So can I start to wash it now, or should I wait for it to settle more?

Timothy
03-31-2008, 03:25 PM
Hi Tilly

If the above is a perfect batch of biodiesel than mine must be the anti-biodiesel because my batch came out exactly the opposite of the above- clear layer (1 inch) on top and cloudy on the bottom.

Tim

Superorb
03-31-2008, 03:34 PM
Originally posted by Timothy:
Hi Tilly

If the above is a perfect batch of biodiesel than mine must be the anti-biodiesel because my batch came out exactly the opposite of the above- clear layer (1 inch) on top and cloudy on the bottom.

Tim
Mine had to sit for a few hours to look like the picture. Right after I shook it up, it looked like how you described, clear on top and cloudy on bottom.

Annatex
04-02-2008, 04:27 AM
Hi All,
I am a new member and I am sick and tired of the fuel price!
Oh I am so over it. $1.50 plus per litre for diesel .That’s it.
I will be going to a small BIO Diesel setup. No question.

I have some books on the way, so I will read them when they arrive.
My understanding from this site is that it isn’t that hard.

Could somebody give me the a rough mix percentage wise, so that I can work out a budget, price per litre?
% WVO %methanol %KOH

I can get my WVO for free and have a price of approx $1.30 a litre for methanol. Is that expensive?

I have a small farm outside of Toowoomba QLD, Australia and would like to initially run my 4WD(turbo) and my tractor.

All help is appreciated

Looking forward to new horizons………some what free of the oil barons!

Cheers
Annatex

Tilly
04-02-2008, 04:39 AM
Hello Annatex

Look at the first post in this thread for the chemicals required to produce a litre of biodiesel. Roughly $0.25 a litre.

How far and in what direction from Toowoomba?

Annatex
04-02-2008, 04:48 AM
Hi Tilly, Thanks for the fast response. I am approx 20Km south of Toowoomba. On Highway.

I did see the 0.25c a lite but cant seem to find rough % to verifiy this. Ie Unsure of the amount to mix. (budget wise only)
How much Methanol per lite of end prodcut being biodiesel? I am assuming amount one fifth. Therfore about the $0.25, is this roughly correct?

Might sound a silly question, sorry just starting out and looking at viability.
Annatex

Timothy
04-04-2008, 02:21 AM
I think I'd dispose of the Draino by using it to clean my drain pipes. Be sure to follow the directions on the can.


Ken, I realize this isn't the venue to discuss this but why would you say that? I't unbelievable that a substance like that is allowed on store shelves for that purpose. Sodium Hydroxide, the same chemical that every biodiesel instruction list is warning you to be so careful around because of it's toxicity? Nothing except water should go down the drain. It's the only thing that most treatment plants can deal with and they don't even do that very well. Heck, our not-so-pristine northern lake is the way it is because of the lack of secondary treatment for plain old sewage. On top of that, it's a totally unnesessary product. I've cleaned 100's of drains using less harmfull methods, never had to pour anything down. These chemicals end up straight in the fish and amphibians inhabiting your streams then in the children playing in the sand at the mouth of the stream entering a lake or in the fish that you pull out of the lake. I WISH PEOPLE WOULD THINK ABOUT THEIR CONNECTIONS TO THE WORLD AROUND THEM! It's not just about the little amount that you put in, it's the cumulative effect of thousands and millions doing the same thing.

Sorry for all that,
Tim

Timothy
04-04-2008, 02:28 AM
Ken,

By the way, thanks for your advice!

Once I get my Landcruiser running again, 5 days and counting, I'll be back to trying another batch.

Tim

Bunk
04-04-2008, 03:54 AM
Originally posted by Timothy:
It's the only thing that most treatment plants can deal with and they don't even do that very well.

If you have any specific information on the environmental impact it has I'd like to see it. I want to do the right thing but I get the feeling you might be overreacting.

Drano claims it's safe in septic systems. Septic systems are an isolated ecosystem of their own and it doesn't seem to disrupt it.
If there is any grease in your plumbing it will be consumed making soap. If it reacts with any acids it will form water and salt. If it reacts with CO2 in the air it forms sodium carbonate.


The Drano MSDS claims "Waste from normal product use may be sewered to a public-owned treatment works (POTW) in compliance with applicable Federal/ Provincial/ State/ Local/ Municipal pretreatment requirements". "All ingredients of this product are listed or are excluded from listing on the U.S. Toxic Substances Control Act (TSCA) Chemical Substance Inventory." "All ingredients in this product comply with the New Substances Notification requirements under the Canadian Environmental Protection Act(CEPA)." I wish lawyers didn't write these things.


Food uses of sodium hydroxide include washing or chemical peeling of fruits and vegetables, chocolate and cocoa processing, caramel color production, poultry scalding, soft drink processing, and thickening ice cream. Olives are often soaked in sodium hydroxide to soften them, while pretzels and German lye rolls are glazed with a sodium hydroxide solution before baking to make them crisp.

Specific foods processed with sodium hydroxide include:
The Scandinavian delicacy known as lutefisk.
Hominy is dried maize (corn) kernels reconstituted by soaking in lye-water. These expand considerably in size and may be further processed by frying to make corn nuts or by drying and grinding to make grits.
Sodium hydroxide is also the chemical that causes gelling of egg whites in the production of Century eggs.
German pretzels are poached in a boiling sodium carbonate solution or cold sodium hydroxide solution before baking, which contributes to their unique crust.
Most yellow coloured Chinese noodles are made with lye-water but are commonly mistaken for containing egg.


So, if we eat the stuff how bad can it be?

Sources; drano.com, scjohnson.com, wikipedia.com.
Ken

rolyat
04-07-2008, 12:55 AM
I did my first Dr. Pepper test today. I don't know if anything happened. I could not find straight NaOH so I used Draino in granule form, which said, "contains lye, caustic soda, sodium hydroxide" I also used the yellow heat bottle methanol. After an hour of setteling it appeared only about the top third of the bottle was biodiesel, and then I thought what if it is just the methonol seperating? So I gave it another good shake, and now it is just chocolate milk colored. Will it settle out overnight, should the cap be on or off, how much biodiesel is usually made from say a liter of oil?
Thank You

Tilly
04-07-2008, 03:05 AM
Hello rolyat

Shake it really hard!

Bunk
04-07-2008, 12:48 PM
Originally posted by Tilly:
Shake it really hard!
Hi Tilly. I tried Drano once. It didn't work for me. I'm not sure any amount of extra shaking will force the reaction. It's a good aerobic workout but that's likely the only good that will come of it.

Ken

Superorb
04-07-2008, 01:21 PM
After drying my BD for a bunch of days, there seems to be some sediment on the bottom. I can't se it until I swirl or shake the jar up. It's light in color and settles to the bottom? What is it, and can I get rid of it by running through a cheese cloth? I'm not going to use this, just sticking in a jar and putting on my desk as a reminder to others that there are alternatives out there.

Tilly
04-11-2008, 09:51 AM
Hello Bunk
I think I missed the "Drano" part.Originally posted by Bunk:
Hi Tilly. I tried Drano once. It didn't work for me. I'm not sure any amount of extra shaking will force the reaction. It's a good aerobic workout but that's likely the only good that will come of it.

Ken

biowill
04-15-2008, 05:00 PM
Hi all,

I have read with much enthusiasm all the posts in this topic. I successfully made my third 1 liter batch with New vegtable oil. I did not however have much luck with some used vegtable oil I got from a local school (with permission of course) I am using magnasol for my washing agent. My question is for the reaction to take place (separating the ffas) does it have to be in an airtight environment? I did use an airtight environment the one liter I successfully made, and the 2 failed attempts I did not.
I am using naoh from Nebraska bio pro.
methanol from a local racetrack. $4.50 a gallon
(50 gal drums)
Thanks ahead of time. And special thanks to tilly for all the useful info he posts.

Tilly
04-16-2008, 09:29 AM
Hello biowill,
Thank you for your kind remarks.

It is best if it is air tight so that no methanol can escape.
Did you titrate the WVO?

biowill
04-17-2008, 02:50 PM
Tilly I am sad to say since my kids go to this school, that it titrated out at 9 for a total of 14.

biowill
04-18-2008, 01:35 AM
Tilly, I also have another question for you if you don't mind. On the NVO before the magnesol wash the ph checked at 9.0, and after at 7.5. However the oil was kinda hazy, so I water washed it and after all was said and done it came out crystal clear. I was actually amazed at the clarity. I also done another batch with the same results. Is this typical of magnesol, or did I just buy 5# of flour as this is what it looks like? Also I checked my titration on the wvo for the 4th time with the same results, and I also done another batch today. It is taking it forever to settle out but a layer at the bottom is forming and mann is it thick. Its a gooey looking white stringy layer.
thanks ahead of time.
biowill

imported_RIT
04-21-2008, 02:48 AM
I have been tinkering with these pesky small batches for a couple of months and I am quite impressed with the success that I have achieved with Saint Tilly's method.

I live on the Texas coast and have problems with drying my small batches due to the sometimes overwhelming humidity. It can take me up to 3 days to dry a small batch in the sun. I recently purchased a small air pump (5-15) gallon aquarium model from wally world (Walmart) to test an accelerated drying process for humid conditions.

I placed 1.75L of cloudy but fully converted bio into a 2L Dr pepper bottle, attached an airstone to about 3 feet of air tubing, dropped the stone into the bottom of the bottle and plugged the unit in.

It only took about 3 hours to dry the entire 1.75L . A possible solution to humidity problems with small batch drying.


RIT


2005 Kubota B7800 running Dr. Pepper BIO at 50%

Tilly
04-21-2008, 10:33 AM
Hello biowill

I have never used magnesol so I can not advise you on that.

"pH is an index (http://www.bentlytribology.com/publications/appnotes/app32.php) of the concentration of Hydrogen Ion (H +) in water. Since oil (biodiesel) is not an ionizing solvent, it has no free hydrogen ions and therefore, it does not have a pH per se. If the oil contains materials which when mixed with water supply hydrogen ions to the water phase, then these will register when the pH of the water phase is measured."

In short, measuring the pH of the biodiesel tells you nothing of importance


Hello RIT
I am glad to hear that things are going well for you!

biowill
04-21-2008, 12:50 PM
ok, thanks for your response tilly. My other batch of wvo that separated was nothing like the nvo glycerin separation. It was a very white stringy substance in the bottom layer. Also I tried to wash part of this batch with water and it would not separate and its been about 4 days now. I also done a glycol test on it and it showed about 50% if that is of any importance.
thanks again
biowill

Tilly
04-21-2008, 01:14 PM
Hello biowill

Did you titrate the WVO?
If you did what was the titration?

Slinger30
04-22-2008, 08:28 PM
If i start out using svo, do i have to heat it up to test? This will be the very first time to see if I'm reading all of this right, "my first test batch" if you will. I'm able to find small amounts of methanol and i'm going to start with that, like I said, this will be my very first time mixing any of this stuff up.

Bunk
04-22-2008, 09:59 PM
Originally posted by Slinger30:
If i start out using svo...
Hi Slinger30. SVO is an acronym meaning "Straight Vegetable Oil". When making biodiesel almost everyone starts with SVO. Do you mean unused or virgin vegetable oil? If it's waste vegetable oil (WVO) what kind of test do you want to do? Free fatty acid? Water?

Ken

Slinger30
04-23-2008, 12:32 AM
Well I was referring to my first test batch of BD just to see how it came out as far as looks, but i went ahead and used wvo i'm waiting for the oil to cool now.

I was going to start with unused oil just to get an idea of what the finished product looks like.

Tilly
04-23-2008, 12:55 AM
Hello Slinger30, welcome ot the forum!

Just to clear it up, SVO does not mean new Vegie oil although some people incorrectly use it to mean that.. SVO is more often used oil and is Oil that has not been transesterfied.

To answer your question, if you are using new oil from the bottle you should not need to heat to remove moisture and you should not need to do a titration..

Bunk
04-23-2008, 02:50 AM
Originally posted by Slinger30:
It don't appear that my first wvo test batch is going to work out, maybe not enough filtration, sooo i want to take some virgin oil just to see how this is supposed to work, i hav 709ml of oil i just bought (for testing) can you tell me how much lye and methanol i should mix for that little bit of oil?

For test batches on new (virgin) oil it's customary to use 200-250 ml methanol per liter plus 5 grams NaOH or 7 grams KOH. To keep the math simple I suggest using 500 ml of the oil and cut the rest of the recipe in half.

Ken

Slinger30
04-23-2008, 12:48 PM
Well I made a test batch and used the virgin oil and it don't look quite right, i have pics of it. I let it set overnight and thought that it should be clearer. can I post pics on here so maybe you could see what ya think? Maybe tell me what i did wrong. I wound up finding 1 liter of oil.

Tilly
04-23-2008, 12:58 PM
Hello Slinger30

It may take several days for biodiesel to clear.

Slinger30
04-23-2008, 01:22 PM
Thanks Tilly, i'll let it set for a few days and see what happens. http://biodiesel.infopop.cc/groupee_common/emoticons/icon_smile.gif

Slinger30
04-24-2008, 03:58 AM
Do you know if it will cause me problems down the road to put all of my collected unprocessed oil in one 55gl drum?? I don't have a filtering setup yet and I need to clean my 5gl buckets to take back to my pickup points.

bernyjb
05-20-2008, 05:09 AM
Hello everybody!

I'm happy to say, I've just been staring at a jar for the last 2 hours, like an authentic idiot.

Finally, after a lot of reading, I just made my first batch, using virgin oil.
However, I didn't quite use the Dr. Pepper technique. After carefully considering the variables posted below:

1) my resources at this time are limited.
2)I have a Harbor Freight scale, which lets me measure tenths of a gram.
3)I have several mayonnaise jars, made from the same PET as soda bottles, but much thicker.

I decided to go with the "Hellmann's" technique, which is like the Dr. Pepper, but making only 1/2 L. batches in a mayonnaise jar.
So I mixed 1/2 L. virgin oil with 125 cc Heet and 2.4 g. NaOH, shook it like the end of the world was coming, and let it settle. As expected, a few minutes later a layer of glycerin started to appear, and so did a smile on my face.
As of now, I'm looking at a very cloudy (as expected) biodiesel layer, and a darker, very clear glycerin layer.

So I'd like to take a moment to thank everybody here from the bottom of my heart, for taking the time to help me, and for ultimately making this a reality.

That said, I have 2 questions:

1) I was expecting the glycerin layer to be about 20% of the total, but I got much less. I still didn't measure it, but I'm guessing about 12 to 15% at most. Is this normal, or should I take it as an indication of an incomplete reaction?

2) In the Dr. Pepper explanation, Tilly said that when using virgin oil the glycerin wouldn't be that much darker than the BD, but I got a darker, very well defined glycerin layer. The BD is very light, almost like the color of the virgin oil, but cloudy, and the glycerin looks like whiskey. Is this normal?

I didn't do a 3/27 yet. I'll probably do it tomorrow (if I can sleep tonight) and I'll post the result.

Superorb
05-20-2008, 12:56 PM
This is the same reaction I got, and it passed the 3/27 test. Good work!

Tilly
05-20-2008, 01:02 PM
Hello berny, congratulations on your success!

The shape of the dr Pepper has been scientifically optomised to make biodiesel, but in a pinch...

The amount of your glycerine layer will vary according to a number of things.
If you use new vegi oil it will be less than if you used waste oil.

bernyjb
05-20-2008, 02:58 PM
Thank you, and thanks all of you for the help. The more time I spend in this forum, the more I realize the kind of frustrations I'd be going through if I had stayed with the "info" from JTF.
Right now, after almost 13 hours, the BD is starting to clear up nicely. And I still can't help smiling every time I look at it. http://biodiesel.infopop.cc/groupee_common/emoticons/icon_smile.gif

bernyjb
05-20-2008, 05:43 PM
Ok, I just did a 3/27.
Actually, I did a 3/27, 4/27, 5/27...all the way to 9/27 (1/3) at 71*F, with no precipitate at all, then I put it in the fridge, where it got down to 50*F, and a ton of precipitate showed up (the liquid was very cloudy, almost like milk), and then I took it off the fridge, and when it got to 65*F I shook it again, completely clear, no precipitate.

Man! WHAT A F#@*&NG RUSH!!! http://biodiesel.infopop.cc/groupee_common/emoticons/icon_biggrin.gif

Ken S
05-29-2008, 12:42 AM
Well it's been about 2 years since I started. Was going good that first summer doing research, getting supplies, etc. Made a test Dr. Pepper batch using virgin oil, worked great. Got real busy with work and other things and dropped the project. Now that $5.15 desiel fuel over Memorial day weekend really hurt. I have reactiviated my project. Have been collecting oil, have about 300 gallons ready to go. Still have not got the big processor, that is in the works. However I am going to start small. Tonight I made my first Dr. Pepper batch with my used oil, it is looking good. One note though, I did not have any clear 2 liter bottles, used a green one from Mountian Dew. I titrated the oil several times using all 3 methods, Phenol Red, Tumeric and phenolpthaleine. Each time it came out between 1.2 and 1.5. I used 6.4g of lye and 200ml of methanol (dry gas). I was getting worried, did not see the separation with the green bottle until I held a flashlight up to the back. Looking real good after 45 mins. I a 6 gallon stainless steel bucket that had something to do with milking, it has a dished out bottom with a center drain, perfect for what I want. I have measured out my 4 gallons of oil and am going to try the first 4 gallon batch this weekend. Thanks for all the good info on this forum.

Tilly
05-29-2008, 05:54 AM
Hello Ken

Good luck on your "Upsized" batch.

UT_Raptor
06-06-2008, 03:27 AM
I found a bad side-effect to TOO MUCH agitation during the one-hour period. I had what appeared at first to be a GREAT looking Dr. Pepper batch, settling and separating just fine. I read too much into the 5 seconds/4 times first hour and did it. It looked so good by the 30-minute mark I put it in the truck to go show a friend. The bumps from driving the truck seemed to break everything up and the glycerin never did settle the same again...so now I need to make a new batch and just use the vigorous shaking method and just leave it alone.

http://biodiesel.infopop.cc/groupee_common/emoticons/icon_mad.gif

Does anyone else have any problems with over-agitation at low speed causing gelling or white floating material in the upper fluid?

Tilly
06-06-2008, 03:40 AM
Hello UT_Raptor, welcome to the forum

Can you be more specific as to what you mean when you said "the glycerin never did settle the same again"
The glycerine should just settle right back out any number of times.

UT_Raptor
06-06-2008, 06:40 PM
Tilly:

Here's what happened...
followed the technique as written and everything went quite well. I feel the only "if" variable was my poor scale which left a big question mark on the actual gram weight of catalyst (soda-lye/drain opener type). After the initial 10-second shake and settle, things were going quite well and progressing nicely. I decided to add in the four, five-second shake idea and shook again once every 15 minutes for 5 seconds each. As you stated, the glycerin settled out each and every time and it did seem that the additional, violent shake seemed to re-mix things and get rid of the foam forming at the top.

So by about 41 minutes into the process, I wanted to take the bottle over to my buddy's house (who helped in the mixing process but had to leave suddenly). Enroute, the bottle simply sat upright on the floorboard. I got to the house only a mile or two away, and as I drove up, the bottle tipped at about the 45 minute mark. I took the opportunity to give it yet another good shake...and at that point, it still settled right back down.

However, I also wanted to show a local gas station owner who was also very excited to see our first go so I put the bottle in a more secure location in the truck and 'headed down the hill.' This is where things got strange...as we were now at the 48:00 - 60:00 mark in the process. I took the bottle out of the truck to go and show and noticed that things were pretty badly stirred up (slow agitation, bumps from the road) but they weren't settling again.

Once I got home, it became obvious that it wasn't going to settle again and even today the upper solution is very clear, but with white floating clouds throughout the solution...and my solid glycerin bottom is markedly less than it was yesterday.

I did another batch, using just your initial hard 10-second shake and sat it in a firm place for the night. Much better results, as this morning I had about 1 inch of settling glycerin on the bottom and the upper part was cloudy liguid (seems normal).

UT_Raptor
06-06-2008, 06:48 PM
Tilly:

in answering a question on the virgin olive oil above, you mentioned several days for the fuel to clear. Do you notice any difference in leaving the bottle out in the sun vs. room temp vs. in the shed/shady conditions? And if so, what do you think the deal is? Heat? Light?

Tilly
06-07-2008, 07:53 PM
Hello UT-Raptor

With refrence to the first post.
I would open the bottle and see if the contents have gelled.
It has been my experience that when using NaOH in the reaction, if you use too much NaOH the contents of the bottle can gel without you realizing it has happened.

In answer to your second post:
That is a tricky question to answer if the biodiesel is not washed. I can not really give you a good answer.

UT_Raptor
06-08-2008, 02:50 AM
I made batch two later that same night, and after several days of settling, everything looks GREAT. So far, the upper layer is cloudy and not crystal clear so I'm giving it another day to settle or clear.

Superorb
06-08-2008, 03:07 AM
^^ It will clear after it has been washed and dried for a few days.

AndyW
06-08-2008, 06:28 AM
This is very interesting. This fellow predicted 4 dollar a gallon gas back in Oct 2007.

http://video.google.com/videoplay?docid=3340274697167011147&hl=en

It appears that there's more to the energy crisis than we thought.

UT_Raptor
06-09-2008, 03:23 PM
Superorb:

Yep...crystal clear after only three hours in the sun venting yesterday but it stayed cloudy until it was washed. Washing went just as Tilly said with gentle agitation at the beginning until about wash 5. By wash 5 the water was relatively clean...although I did notice more foam and bubbles in the water layer with the harder agitation. I also noticed a slight drop in yield after the wash.

Superorb
06-09-2008, 03:46 PM
Slight drop in yield is normal. Good job http://biodiesel.infopop.cc/groupee_common/emoticons/icon_smile.gif When I left cap off to vent, dust settled in mine. I had to strain through a coffee filter. I've got a jar sitting on my desk at workhttp://biodiesel.infopop.cc/groupee_common/emoticons/icon_wink.gif

UT_Raptor
06-14-2008, 01:05 AM
Well, just when you think you've got it, then you try a dirty oil 2 liter bottle and get SMOKED. http://biodiesel.infopop.cc/groupee_common/emoticons/icon_razz.gif

I don't have my titration kit so I thought I'd be clever and get the guy who gave me the old oil to do the titration. That's all good except he has KOH and I have KaOH(?). I remembered that it took 63mL per the test so I plugged that number in and attempted to use THAT result to and use MY catalyst. BIG mistake.

The stuff never did 100% dissolve in Methonol and as soon as I poured this mixture into the oil it all coagulated in a big, marbled nightmare! It looks like a brown-sugar/oatmeal explosion in a 2-liter bottle.

SO I guess the obvious fix is titrate using KaOH since that's my catalyst and go with THOSE numbers, not the KOH numbers. Still kind of funny (by the way, does 70 grams of soda lye sound like a lot for 1 liter of WVO?).

Tilly
06-14-2008, 01:13 AM
Hello Raptor

Do you mean 63ml or 6.3ml

An NaOH titration of 6.3 is on the high side and likely to give you problems.

UT_Raptor
06-14-2008, 03:44 AM
It took several full pipettes plus 3 (ml?) on the final which seemed to yield a total of 63 units. I thought it was ml of suspension and then you divide that number by 4(?). Again, I didn't do it myself but merely recorded the result. Chalk it up to me being lazy.

But yes, it took quite a bit more solution to turn and hold color compared to a new batch that I watched him do last week.

UT_Raptor
06-14-2008, 04:05 AM
Originally posted by Tilly:
Hello Raptor

Do you mean 63ml or 6.3ml

An NaOH titration of 6.3 is on the high side and likely to give you problems. Yep, I screwed up and screwed up BIG. The end result of 63 ml of solution was based on FOUR ml of test oil, not one. The end result, 63, MUST be divided by 4 and then added to the base amount. I should have used somewhere in the neighborhood of 19 grams of catalyst and instead attempted to introduce SIXTY EIGHT GRAMS.

I have successfully made a batch that looks like oatmeal mixed with brown sugar...kind of like a "ship in a bottle."

As promised, photos of the ugly, the bad, and the good...

http://www.flickr.com/photos/83123420@N00/sets/72157605...how/with/2582954730/ (http://www.flickr.com/photos/83123420@N00/sets/72157605632594380/show/with/2582954730/)

UT_Raptor
06-17-2008, 09:56 PM
Originally posted by UT_Raptor:
Superorb:

Yep...crystal clear after only three hours in the sun venting yesterday but it stayed cloudy until it was washed. Washing went just as Tilly said with gentle agitation at the beginning until about wash 5. By wash 5 the water was relatively clean...although I did notice more foam and bubbles in the water layer with the harder agitation. I also noticed a slight drop in yield after the wash. follow on to this was that I should have let the post-wash settle much more than I was after violent agitation. Next time around, I will allow much more time for settling after washes 4 and 5.

I also noticed that Tilly's method of ONE 10-second shake using WVO seems to work far better than the 5 second shake every 15 minutes. I had good separation after the first 10 second shake and should have left it at that (see pics above) but I wanted to test the 15 minute interval agitation to see if I got better yield. Instead, I once again got somewhat of a congealed mess as I did with SVO. Catalyst could also be the culprit, as the scale I'm using isn't as accurate as it should be.


But this does leave a big question for me...once I nail down the catalyst and period of agitation to produce acceptable fuel how should I interpret those results towards use in an Appleseed? I ask because it would seem that with pump agitation that I may have the same problem as I did using the 15 minute interval shake...where one violent shaking period yields good fuel while intervals seems to mess things up a bit.

imported_belugas
07-06-2008, 09:47 PM
Hello-

I just ran my first ever batch (Dr. Pepper method) using wvo I got from my brother in law who is a chef. The fryer oil he gave me was quite dark, about as dark as doctor pepper, it has been sitting for about an hour and all I can see is about 3/4" of somewhat clear fluid on the top, the remainder is as dark as it started.

I have not found any info on dark oils in your forum or in the DR. Pepper Method pages. Do I need to go to a wvo forum? Or can someone help in this forum? Should I do a titration or is this oil simply burned or to full of FFA'S or did I mess up somewhere?

I followed the dirctions for the WVO ...it has been sitting for a few weeks after I filtered it with a 100 micron mesh filter.

Thanks-

Belugas http://biodiesel.infopop.cc/groupee_common/emoticons/icon_rolleyes.gif

Tilly
07-07-2008, 12:13 PM
Hello belugas, welcome to the forum

Hold a light behind the Dr Pepper Bottle and see what it looks like

imported_belugas
07-09-2008, 02:25 AM
Originally posted by Tilly:
Hello belugas, welcome to the forum

Hold a light behind the Dr Pepper Bottle and see what it looks like

Thanks for the welcome-
with a light behind the bottle, the bottm half inch is a white sludge, the next 6" layer is dark coke color liquid, the next layer is a paper thin layer of a tan precipitate, and the top layer is light amber clear layer about 1" tall.

When I heated the oil I might have over heated it a bit because it did smoke a bit. Also, my wvo starts out as dark as root beer. No titration yet.

What you think?

Thanks-

belugas

Tilly
07-09-2008, 04:02 AM
Hello belugas

I suspect that you have some high titration oil and you will need to do a titration

anthony111
08-01-2008, 12:19 PM
Hi all, did my first test sample yesterday using new oil, i got seperation almost stright away. I shook it for 20 sec quite hard, is this too much?. i now have BD with small white bits floating around and the stuff on the bottom is a light brown colour, also my BD is cloudy but think i may of shook it to much. do i need to leave it longer to clear up, or do i need to wash it. i used 6g of sodium hydroxide any help anyone ....... thanks in advance

anthony111

gulfy
08-02-2008, 02:44 AM
Hi all. I too just finished my first test batch using new oil. I followed Tilly's Dr.Pepper method to the letter. After shaking a dark amber liquid settled to the bottom. I removed the glcryn and did the water washes. The top fuel was cloudy and the water was cloudy also but got more clear after each wash. After the last wash the water was almost completly clear. I set the fuel out in the sun with top off and after about an hour it turned crystal clear. It did have two small droplets of water remaining in the bottom, but still after two days the fuel is crystal clear..I'm very happy with the results and getting ready to try it again..thanks again to Tilly and the Dr. Pepper method...

doggiedoc
08-22-2008, 01:03 AM
Hi all! Still making test batches here to get tthe feel for everything. I've start #5 tonight with some real WVO this time. It titrated to 3 so I used 8 grams of NaOH for my methoxide mix. http://biodiesel.infopop.cc/groupee_common/emoticons/icon_biggrin.gif So far so good. This stuff is dark!!

So I do have a question (or three.) I has been stated that shaking 4 times for 5 seconds over an hour is better than 20 seconds at the beginning of the reaction. Is it possible to shake too much? What about constant mixing after the vigorous shaking? Will that help or harm the batch or is there no need?

Thanks in advance!
Doc

Tilly
08-22-2008, 01:20 AM
Hello doggiedoc

The more mixing the better.
You need to keep periodically shaking to keep the chemicals in the reaction area. If they are allowed to settle out then the reaction will stop early

doggiedoc
08-22-2008, 01:27 AM
Saint Tilly -

Thanks for the fast response but now you've confused me. The reaction doesn't start until settling? I assumed it was taking place right away during the first mixing.

Am I confused?. Please clarify.

Thanks,
Doc

Tilly
08-22-2008, 01:50 AM
Hello Doc

I was typing too fast and did not check what I wrote.
It should have been STOP early.

doggiedoc
08-22-2008, 02:21 AM
Ah, thank you kind Sir for the clarification!

http://biodiesel.infopop.cc/groupee_common/emoticons/icon_biggrin.gif

dr1step
09-27-2008, 05:56 PM
Hello all, I'm a newbie at BD and forums in gerenal. Usually to stubborn to ask for help! Ha! Anyway I 've been reading for about 3 months about all this stuff and decieded to take action. I've built my own wvo collection tank and put collected the parts for my processor. So last week I made my first liter batch using the Word Famous DPT. It came out OK, not that clear and not as yellow as the picture on this forum. So I decieded to process it again. Boy did I do something wrong!! I ended up with something that looked like marble with the consistancy of jelly. OK things I didn't do the second time. Didn't titrate. Used the same Meth/lye measure as first time. Heated reprocessed oil to 212 deg. to cook off any water. Let cool to 140 +- 5 added meth/lye turned to mild emedately!
Thats not the end... Did another batch the next day. Told myself I was going to try the 80/20 method. Again the first 80% batch went well. After an hour good seperation but cloudy and brown not nearly yellow and clear. Then I heated the BD up again to 212+ to cook off any suspended water and meth, let cool to 140+-5 then added the rest of my meth/lye mix. Cap tightly and mix vigorusly let rest over night. Vola - clear gelly??????? What the %^#*@ ! Am I missing something?
_________________________
To stobborn to know better

Bunk
09-27-2008, 06:24 PM
My guess is that you used too much NaOH causing the gel to form. Also, don't boil off the methanol between the 80/20 stages.

Ken