nightmare batches!!!

[dgs]

Titration fluid is only a few weeks old

Blank the solvent??

The earlier 27/3 test does appear cloudy, but I had this with the ones I did on the previous nightmare batch, which went clear later on.

On the 270/30, the mix in the bottle part looks cloudy but the syringe is clear, I can read the markings easily through the syringe

Leave it until the methanol phase is clear, then check it. Tubes are £38

[countrypaul]

If you are using IPA as the solvent for titration it canbe acidic. Normal practice is to therefore put the solvent in the container to be used for the titration, add the indicator and titrate untl you just get a colour change that way you know there is no acid left from the solvent. You then add the oil which will normally change the colour back before carrying out the titration of the oil.

[Vijay]

Titration fluid is only a few weeks old

Blank the solvent??

The earlier 27/3 test does appear cloudy, but I had this with the ones I did on the previous nightmare batch, which went clear later on.

On the 270/30, the mix in the bottle part looks cloudy but the syringe is clear, I can read the markings easily through the syringe

Leave it until the methanol phase is clear, then check it. Tubes are £38

Will do.

What size are they? Do they do 90/10 or larger?

[Vijay]

If you are using IPA as the solvent for titration it canbe acidic. Normal practice is to therefore put the solvent in the container to be used for the titration, add the indicator and titrate untl you just get a colour change that way you know there is no acid left from the solvent. You then add the oil which will normally change the colour back before carrying out the titration of the oil.

I do use IPA but have never blanked the solvent in the past but can do if you think it would help?

[dgs]

You can get separating funnels that are larger but they don't have the graduations where we need them, so 10/90 is  what we use.

[dgs]

If you are using IPA as the solvent for titration it canbe acidic. Normal practice is to therefore put the solvent in the container to be used for the titration, add the indicator and titrate untl you just get a colour change that way you know there is no acid left from the solvent. You then add the oil which will normally change the colour back before carrying out the titration of the oil.

Why would putting the ipa in the container to be used for the titration make it go alkaline Paul. Unless we make it alkaline we can't titrate to blank it?

[countrypaul]

If you are using IPA as the solvent for titration it canbe acidic. Normal practice is to therefore put the solvent in the container to be used for the titration, add the indicator and titrate untl you just get a colour change that way you know there is no acid left from the solvent. You then add the oil which will normally change the colour back before carrying out the titration of the oil.

Why would putting the ipa in the container to be used for the titration make it go alkaline Paul. Unless we make it alkaline we can't titrate to blank it?

Maybe a confusing use of the word container.  I normaly use a concical flask for titrations, but I thought that may not be used by everone.  Just putting the IPA  in the container would not make it go alkaline (unless it was contaminated).

What I meant was put the IPA you normally use into the conical flask (or whatever you use) add the indicator and then neutralise any acid present in the IPA by adding alkali as similar to normal when titrating. As soon as the indicator changes colour stop then add the oil and titrate as normal, much as suggested: https://biopowered.co.uk/wiki/Titration

I was merely highlighting that IPA can often be acidic so neutralising it before adding the oil will give a more accurate titration figure for the oil.

[Vijay]

Left the 270/30 test overnight but found that some of the unconverted oil was kinda sitting in the lid (where I wouldn't get it in a proper coned flask). I kept tapping it and gently turning the bottle allowing anything to hopefully sink into the syringe. So it looks like I've ended up with 0.3ml at the bottom. I'd assume this is a good conversion, so how come no glyc?

[dgs]

Left the 270/30 test overnight but found that some of the unconverted oil was kinda sitting in the lid (where I wouldn't get it in a proper coned flask). I kept tapping it and gently turning the bottle allowing anything to hopefully sink into the syringe. So it looks like I've ended up with 0.3ml at the bottom. I'd assume this is a good conversion, so how come no glyc?

besause you have used biodiesel so although there will be glyc (a small amount, max about 0.3%) in the bio it dissolves in the methanol so invisible to the test.

Yes, well done its a good conversion.

[Vijay]

Left the 270/30 test overnight but found that some of the unconverted oil was kinda sitting in the lid (where I wouldn't get it in a proper coned flask). I kept tapping it and gently turning the bottle allowing anything to hopefully sink into the syringe. So it looks like I've ended up with 0.3ml at the bottom. I'd assume this is a good conversion, so how come no glyc?

besause you have used biodiesel so although there will be glyc (a small amount, max about 0.3%) in the bio it dissolves in the methanol so invisible to the test.

Yes, well done its a good conversion.

Great   So where's all the glyc and how do I get it out lol  No glyc dropped when I did the batch and then I added an extra 40l or so more glycerol -  but nothing has dropped.....................

[dgs]

I'm confused here, on post No 56 you reported that the glyc had dropped.

[Vijay]

I'm confused here, on post No 56 you reported that the glyc had dropped.

Post 64 mate lol   "Moved back onto the previous batch that went wrong. IIRC it titrated at 8 so added 1200g Naoh and 18l meth. No glycerol dropped. So today I got everything back into the processor with extra glycerol, mixed for 30 mins at 50c and took a sample. No glyc has dropped. Where do I go from here with this batch?"

As the advice worked for the batch I posted about, I tried the same advice for the previous batch that had failed (no glyc dropped). The 27/3 and 270/30 test pictures I posted are from this batch which I have not been able to drop glyc from.

[countrypaul]

So just to make sure we all have the correct understanding, this is the last but one batch that went wrong. You had 85L of oil that titrated at 8 so added 1200g Naoh and 18l meth. There was not glycerol dropout you you added 40L more glycerol and still not dropout but testing it gives what you are showing in you home made 10/90  or 30/270 tube?

If so that makes very little sense to me. You basically have about 80L of bio that should have about 60L of glycerol in it, yet there is next to nothing in the tube but no glycerol has dropped out?

Are you sure you added the oil from the failed batch and not the bio from the last batch? Are you sure you tested the mix from the failed batch and not the bio from the successful batch?  Sorry for the questions, but the evidence doesn't all appear consistent to me.

[Vijay]

So just to make sure we all have the correct understanding, this is the last but one batch that went wrong. You had 85L of oil that titrated at 8 so added 1200g Naoh and 18l meth. There was not glycerol dropout you you added 40L more glycerol and still not dropout but testing it gives what you are showing in you home made 10/90  or 30/270 tube?

If so that makes very little sense to me. You basically have about 80L of bio that should have about 60L of glycerol in it, yet there is next to nothing in the tube but no glycerol has dropped out?

Are you sure you added the oil from the failed batch and not the bio from the last batch? Are you sure you tested the mix from the failed batch and not the bio from the successful batch?  Sorry for the questions, but the evidence doesn't all appear consistent to me.

Yep absolutely correct.

I'm 100% certain that it's the batch I made in the last but one. It was labelled up and put in a shed out of the way when I removed it from my processor.

100% certain it's not the bio I made in the last batch. That is sitting in a settling tank

[Vijay]

is it worth trying more glyc? maybe do a sample with more glyc?