well i tried the acid stage about two weeks ago
for the first time, ive been making bio for a year
i used this recipe koh is used
31 gal (117.3L) 3.1 gallons methanol
titrated 8.1
target 3
8.1-3=5.1
5.1x0.2=1.2ml per liter

1.2x117.3=140.76ml of sulfuric acid
mix into 3.72 gallons of methanol (60%)
react a 140*
do titrations every hour untill 3ml is acheived
leave on pump(6hrs)( settle 12hrs)

well it never fell untill the next day it went to 9.1 then the day after that to 7 and it stayed at 7 for a week then i stopped messing with it because i got busy now two weeks has passed and i got some time to mess with it. i pulled out a sample and this time i let the white clumps settle before the titration and i got 5.5, 5.6 and 5.5 my question is that is it the white stuff throwing off the titrations and can i reheat this and kick start the process to get down to 3. the oil is 80* F will the methanol blow me up if i turn on the element. i use an appleseed processor here is a pic of the white stuff. also there was an immense vac created as the reaction cooled over a few days just curious.


thanks all

rhino
-looks like the wvo was wet,this will end the esterfication process before minimum T is reached! also, the ae process will stop if the temp is not maintained, to restart, reheat. Tom

Rhino,
Do the white clumps look like large granular chunks of salt a little smaller than rock salt? If so I would suspect it to be Potassium sulfate or Sodium sulfate that results from the sulfuric neutralizing the caustic that was in the processor from the previous base stage. Water heaters aren't the best at completely draining. If this is the case then adding more sulfuric may be all that is needed.

so how much acid should i add and how much methanol? thanks for the input

the chunks are not grainular there more like gooey clumps that take a couple mins to settle

Rhino,
If it were me, I would run the pump to thoroughly mix the contents of the processor. Then pull a 1L sample out for a mini batch. To this sample I would add .5ml of sulfuric (erring on the low side not the high), heat to 140F, shake every 15 minutes or so just like any other mini batch. Check the T after about 2 hours (immediately after shaking) and see if there's any change. If there's no drop in titration, then I'd try something else.

well i reheated the mix to 140 and added 40 ml of acid and 1 gal methanol to try and kick start the process. it has mixed for 2hrs and titration went from 5.5 to 5.8 it did lose 8 deg F tho so i will heat back up

update T is now 5.1 hopefully it will continue to fall. ? should i keep heat on it the entire time weather the pump is on or off

Well ain't that a SOB.
I thought you said it was a T7 while the white chunkies were stirred up. Did you titrate this last time with the white chunkies stirred up?
If you draw a sample out of the processor the same size as the one in the picture and allow it to settle after titrating, is there more white sediment or the same amount?
I'm wondering if the T will lower just with more of a run time?

the chunks do not appear while it is hot so i titrate as soon as i pull a sample but it is getting lower so i am doing something right

Thanks for the update Rhino.
keep us posted on what is titrates tomorrow or later tonight.

i got it down to 5.0 then added 2.5 gal methanol and 50 something ounces of KOH and processed some good bio thanks for all help i will dry my oil next time