Hello to all,

I made today my first test batch of 4 galons of WVO. The oil tritated at 3 (tritated 3 times). I use a base of 7.5 for KOH which totals to 10.5. I used 159 grams of KOH and 20% methyl alcohol. This filled a 5 gallon carboy. I mixed it for a minute and let it sit. 8 hours have passed and I see absolutely no seperation.

What did I do wrong??

Hello prpony, welcome to the forum
Are you sure you did not get seperation?
If the sides of the container are not translucent it is hard to see.
While 1 minute of mixing should give seperation, you do need to mix longer If you wanted to make biodiesel that passed the 3/27 test

Welcome to the forums: prpony

Your ratios sounded just a little short, but the jug was too full to mix very well. And 30 minutes is about the minimum.

If you didn't heat the oil up to about 120 to 130 degrees F it will react vey slowly.

It will contunue to react even at room temperature, so give it a week and see what it does.

Read alot in these forums and you'll get it figured out.

Goodluck

Hello prpony
How did you mix it?

Hello PGBiodiesel

quote:

Originally posted by PGBiodiesel:
If you didn't heat the oil up to about 120 to 130 degrees F it will react vey slowly.
It will contunue to react even at room temperature, so give it a week and see what it does.

A week! Wow, that would be really cold!

Unlike the acid stage of an Acid/base procedure, once you stop mixing the single stage reaction, the reaction stops as the glycerine settles to the bottom.
To continue the reaction over the week requires that you continue to mix over the week which is likely to be a bit excessive.

quote:

Unlike the acid stage of an Acid/base procedure, once you stop mixing the single stage reaction, the reaction stops as the glycerine settles to the bottom.

Of course I disagree with you Tilly. It does need more mixing, but not to bring the glycerine back up but to bring the methoxide down into the oil.

The methoxide is thinner and lighter so floats on top of the oil. And very little glycerine has been produced to carry any methoxide down with it.

If a person could shake 5 gallons of mixture in an 8 gallon container as vigourously as you do with a little pop bottle for one minute then it might work.

Hello PGBiodiesel
If you will look at my first reply I pointed out that a minute is not enough mixing time.
I can not guess how he mixed his batch or how violent his mixing was. For all I know he might have used a Paint stirrer in a drill.

But your advice that "It will contunue to react even at room temperature, so give it a week and see what it does." Certainly does not even come close to what I have experienced.
If his initial mix was not sufficent to even mix the methoxide thoroughly as you seem to be suggesting then waiting a week will accomplish nothing other than possibly forgetting where you put the container

OK, I mixed it by Dr. Pepper method. I let it sit until 3pm today, more than 24 hours and absolutely no seperation. I assumed the carboy was perhaps too full so I did a a new batch with 3 galons instead of 4. I tritated at 5 + 7.5 base = 12.5 which gave me 159 grams of KOH. I added 2% more of Methyl Alcohol to 22%. I shook it for 3 minutes. I do not heat the oil because it is 93 degrees in the shade here right now.

What do think?

ohhh... and no seperation on the new batch either. I do notice a top layer of about 2 inches which I think is the Methanol.

Hello prpony

The initial mix should be as Viokent as possible.
If you are "Shake" mixing as in the Dr Pepper procedure you do need to leave head space to insure the liquid can splash around violently.

If you have a layer of methanol on the top of the oil this is a good indication of insufficent mixing vigour.
If you look at This video at around the 2min 40seconds it shows washing biodiesel in a drum with vigerous mixing action.

I think you should have started with a 1 litre batch in a two litre Dr Pepper bottle.

Thanks Tilly,

I did make a liter once before and it did seperate very well. I think you are right, I will make a third and shake much more agresively.

I will let you guys know.

Thanks.

And leave lots of head room in the reactor

If lack of mixing vigour is the only problem, your other batches should be salvagable too.

OK, now I am about frustrated! I did another 3 galon batch earlier today and shook the heck out of it, my two brothers and I took turns. AGAIN, no seperation......????

I thought maybe it was the oil.. it sat outside in the sun for a month in 5 galon carboys. So I went a got fresh oil from one of my suppliers and did a tritation which it tritated at 1. so.. 22% meth, 97 grams of KOH and did another 3 galon batch and.... NO SEPERATION!!!

Perhaps I am tritating too low..??

This is my tritation set up;

10 ml. lye= 1 gram of KOH (90% potassium hydroxide) in 1000 Ml. of distilled water.

3 drops= 91% phinophalein (or something like that)

10 ml.= 91% Isopropyl Alcohol

1 Ml.= oil from source


What can it be?

Hello prpony

Just to be sure, when you titrated, it took 1ml of the Lye water to turn the alcohol/oil pink or did it take 10ml?
Did you check for water in the oil?
Put a small amount of the oil in a pan and heat it. If it starts to snap or pop as it approaches 100deg C it is water.
If there is no popping up to 110 and all you see is convection currents in the oil that suggests no water.

Be careful because water can spit hot oil all over.

Things I think can be...

I did not use a .01 gram scale to do my Lye.. I used a gram scale where the gram could have been 1.9 for all I know.

I do not heat the oil, It is 93 in the shade here. Could it need more heating to react??

My Potassium Hydroxide is 90%. Is this fine?

These are the only unkowns.

quote:

Just to be sure, when you titrated, it took 1ml of the Lye water to turn the alcohol/oil pink or did it take 10ml?
Did you check for water in the oil?
Put a small amount of the oil in a pan and heat it. If it starts to snap or pop as it approaches 100deg C it is water.
If there is no popping up to 110 and all you see is convection currents in the oil that suggests no water.

Be careful because water can spit hot oil all over.

Saint Tilly

It took 1ml of the Lye water to turn the alcohol/oil pink

I will do the water test now.

I heated 30 ml of oil at 100C, no popping and I continued heating until it started burning and no popping. Just very fine bubbles in the beginning. I still have 30ml. of oil.

Hello prpony

quote:

Originally posted by prpony:
I did not use a .01 gram scale to do my Lye.. I used a gram scale where the gram could have been 1.9 for all I know.

We are only talking about a titration of 1. Even if your titration fluid was off you should have at least achieved seperation.

quote:

I do not heat the oil, It is 93 in the shade here. Could it need more heating to react??

As long as everything is liquid, temperature is not a limiting factor. You should have achieved seperation at 93deg F.

quote:

My Potassium Hydroxide is 90%. Is this fine?

Yes, just increase your "Base" amount to 7.8 to compensate for lack of purity. Your use of 7.5g KOH base would not have prevented seperation.[/QUOTE]

what did you mean when you posted above;
"10 ml. lye= 1 gram of KOH (90% potassium hydroxide) in 1000 Ml. of distilled water."

quote:

what did you mean when you posted above;
"10 ml. lye= 1 gram of KOH (90% potassium hydroxide) in 1000 Ml. of distilled water."

My seringe was full to 10ml. so to measure ml. used in tritation and that this lye was made with one gram of KOH to 1000ml of distilled water.

This is really embarassing. I have invested about $4,700 in equipment to produce 200 galons a day and am currently collecting almost 1000 galons of WVO a week and I can not even get a 3 galon batch going. The first time I did a litre was so easy and flawless, I bragged to my friends and now that I am ready to produce my first 200 galons I get stuck.

Hello prpony

Are you using different chemicals than you used to make the original test batch?

when I first did the liter test batch I used Heet and a drain declogger, I forget the name of it but it had high concentration of potassium. Now I am using the real chemicals as mentioned before. When I do the Methoxide it gets very very hot. I assume the methanol and potassium is fine because of the reaction and the time it takes to disolve.