I am attempting my first batch using the acid/base method. I mixed up the sulfuric and methanol last night and mixed for three hours. Titration dropped from 18 to 13 at the end of three hours. I let it set overnight and this mourning it had dropped only to 12.3.

The temperature this mourning was 125 so I started to heat it back up to 145. That was when I noticed I have a small vent leak (I could see steam) and now I do not know how much methanol I have lost. I did have a thin layer of what I believe to be the meth/water layer on top this mourning.

Any ideas on what I should do at this point?

I would suggest you keep mixing...
if the titration reaches 7.stop..

you didn't mention if your're using KOH or NaOH for titration...

if KOH.. drain about 1/2 of the amount of methanol you starter with. remix and recheck the titration.

depending on how much methanol you started with.. what's on top might be BD or methanol?
did you start with 12%( of the oil volume for methanol?)
are you using KOH for titration? is this 1% or 0.1N solution?


-dkenny

Hi dkenny, I am using koh and at 1% for titration. I also am using your formula for the acid/base process. And the top of it may have been biodiesel, it "looked" like it.

if it did what it was supposed to do..you do have BD on top. the water/methanol/acid should be on the bottom.

keep mixing for a while longer may 5 hours more then recheck the titration while its mixed.

after it reaches 7 then settle for 12+ hours. might not actually take that long but I know 2 hrs isn't enough.

good luck

-dkenny

Thanks for your help dkenny. I waited till it titrated at 10 and went ahead processed. This was after mixing and settling for two days. I did the 27/3 test and it did not pass so then reprocessed and it barely failed again. I am fixing to reprocess again and hopefully this will do it. Then I can try another batch and hopefully get it right on the first try!