Problem with batch

[NornIron]

Hi all, new to this forum, I'm usually on the VOD but as it's down I thought it would be the perfect time to sign up here. I know Julian as he helped me greatly with my PID set up so hopefully he'll be along to say hello.
 

Don't know what's going on with my second batch but hoping for some advice. The sample jar on the left is after 1 hr processing and the one on the right is after 1.5 hr. I have no conversion with a 90/10 test.
 
It was a 180L batch and this was the 1st stage. I have dropped about 45 litres of glycerol which seems an awful lot.
 
I've got a feeling there's something up with the oil as it looked really murky even after the glycerol pre wash and I believe this is supposed to clean up the oil?
 
I'm concerned it was still wet but I had it heated to 70 in my drying tank and bubbled it for a few hours. I then added the glyc and transferred to the processor, ran through for 1/2 an hour, drained glyc and used the venturi and condenser to dry further. I took over 4 litres of water out through the condenser. 

[RichardP]

To me that looks like it was caused by wet oil. Your drying method seems a bit back to front, you should really dry it with the venturi first, then, when there's no more water coming off, do the glyc wash. You won#t need to bubble if you use the venturi first.

[NornIron]

I'll have a look at my drying method for the next time as I think I've got a bit confused. The problem I had which I have learned since was that I was trying HPT tests after I added the glyc, which obviously does not work due to the methanol present and the methanol was bubbling.

What I really need help with is what I can do now? Is my only option to start stage one again?

[julianf]

It looks like you have a glycerol layer there?

If so, you must have some conversion, otherwise there would be nowhere for the glycerol to come from (unless the glyc wash was improperly drained)

I would drain whats there, re-do the 90/10 test, and cautiously proceed, either according to the test results, or, if you really have no conversion, add a small amount more meth (say 7%) with, say, 3g /ltr and see what happens then.

[NornIron]

Thanks Julianf, yes, there is definitely a layer there.

It's been sitting over night so I'll drain down anything that's left and do another 90/10 and see what that says.

[RichardP]

And do a Dr Pepper after that to see how much meth/catalyst you need.

[Julian]

Hi, welcome to the wiki and forum.

I'd pretty much agree with the advise to date.  4ltrs of water is quite a lot to recover from 180ltrs of oil.

It does sounds like the problem was insufficiently dried oil.  To recover this batch try adding additional methanol and catalyst to a sample.  Easiest way to prove the point is to take a small sample and overdose it.  If that works you know it's possible and can do 3/27s and Dr Peppers to find out the exact quantities.

For future batches, I'd forget the glycerin wash until you've perfected the basics.  Dry the oil really well using the venturi at around 85 - 90°C until no more water comes off.  Then just do a simple two stage with titration.

Start with the basics and get that off pat, then try all the fancy stuff if you want.  I've tried most things but still do a simple two stage with titration as my preferred method.

[rbdazza]

Deffo wet oil. Been there got the t shirt. If it were me I'd go for full stage 1 catalyst again with the least amount of method you can mix in. Noah for me for instance it'd be 800g and 8l of meth.

[NornIron]

Ok, wasn't so sure on that Dr. Pepper test so I did a micro test with 180ml of the bio heated to 55-60 degrees, added 7ml methoxide (from 1st stage, 5g base NaOH) and shoke the heck out of it. I then did a 90/10 on this and it shows that I would have 6ml drop out which is 60% unconverted which is 108 litres. At least the second stage is showing a reaction.

I have went with methoxide mix based on this for second stage and after mixing am now showing 35% unconverted oil. Will continue tomorrow, have drained down the gycl.

Yes, Julian, I think I'll leave that glycerol pre wash next time until I get the basics nailed, thanks.

[Tony]

Half the skill is learning how to recover batches when it all goes a bit wrong.  Sounds like you've got it under control - just chalk it up to experience!

[rbdazza]

have you finished it off?

for your next batch, do a search on here and VOD for drying veg. its been discussed loads of times. some say its the most important step of making bio, your search results may well be drowned out by some old fella who goes by the name of Jim. he reckons drying your oil is pretty important too...

just remember, the glyc wash is a fail safe, it takes any remaining water out and passes on any chemicals it carries to your oil as a brucy bonus. the idea is your oil should be pretty much dry by the time you do it.

[NornIron]

Oh bugger, I think I've got a big problem. I ran out of time last night so I drained the glyc down after stage two and I left it with the intention of doing stage three this evening after work. I have just done three and this is what's in the tank?

I've got a nasty feeling that I'm not supposed to leave NaOH overnight?

Any advice please?

[Julian]

Still looks like soap.

Try filtering (J cloth or similar) or settling it and see what the bio is like ... 3/27 test again.

At what did this oil titrate?

[NornIron]

I'll get it into the settling tank then, I am very worried about having this in the processor.

I didn't titrate it, I don't have the gear to do that. I didn't think it was relevant anymore after the two stage process was introduced, I am now finding after the problems I am running into on my first batches that it is very relevant and why.

I will transfer it and then give a bubble over night do you think? I can see what it's like after that and if I can get the soaps all out then I could consider re processing as well?

[NornIron]

This is settling out, albeit I have created a shed load of soaps. Could this be caused I have overdosed the NaOH?

I have been concerned on my calculations with the batch as the oil was so bad and I have made loads of glycerol that my true batch size was probably a lot smaller than I calculated which in turn means that the my NaOH amount on the unconverted oil was incorrect.