Author Topic: nightmare batches!!!  (Read 13524 times)

Offline Vijay

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Re: nightmare batches!!!
« Reply #15 on: August 04, 2022, 09:33:00 AM »
I'd like to try option 3 as I'd love to see this batch through and learn.

So for 85l of this oil mix, if I add 20l of glycerol at a time, how much sodium and meth would I mix for the methoxide?   Should I do some 1l samples of this or do the 85l in the processor?

Offline countrypaul

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Re: nightmare batches!!!
« Reply #16 on: August 04, 2022, 12:06:41 PM »
I would definitely do some Dr Pepper experiments rather than jump in at the deep end with the whole batch.

Follow Dave's suggestion of adding enough caustic to neutralise the FFA in the minimum amount of methanol you can get away with.

For 1 1L test, I would try 12g of NaOH (or 16g KOH if you have it) and I would start with 50ml methanol. Be warned adding 12g NaOH to 50ml methanol in one go may make the methanol boil so add 3-4g at a time and check how warm the solution is once dissolve then allow it time to cool. Mixing the methoxide dont use a PET container (soft drink bottle), use an HDPE/MDPE/LDPE one or glass as methoxde will dissolve its way through!

One treated and the glyc removed, you should be able to use 5g NaOH/200ml methanol to process the test -youmay need a second step with the processing to remove the last of any dropout.

Offline Vijay

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Re: nightmare batches!!!
« Reply #17 on: August 04, 2022, 12:13:25 PM »
"For 1 1L test, I would try 12g of NaOH (or 16g KOH if you have it) and I would start with 50ml methanol. Be warned adding 12g NaOH to 50ml methanol in one go may make the methanol boil so add 3-4g at a time and check how warm the solution is once dissolve then allow it time to cool. Mixing the methoxide dont use a PET container (soft drink bottle), use an HDPE/MDPE/LDPE one or glass as methoxde will dissolve its way through!"

so mix 12g/50ml with how much glyc to do a glyc wash?

I do have some pot, so recommend using that over sodium?

Offline Vijay

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Re: nightmare batches!!!
« Reply #18 on: August 04, 2022, 12:14:34 PM »
"For 1 1L test, I would try 12g of NaOH (or 16g KOH if you have it) and I would start with 50ml methanol. "

so mix 12g/50ml with how much glyc to do a glyc wash?

I do have some potassium, so recommend using that over sodium for high titration?

Offline RichardP

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Re: nightmare batches!!!
« Reply #19 on: August 04, 2022, 12:50:19 PM »
As Dave says I did mean 1g/l in a liter of meth once the glyc was in and washing. I've only had to do this on a few batches some years ago when I had some real crappy oil that titrated around 7 with sodium. Any soapproduced would have come out with the glyc and they processed well afterwards, thought the final volume was a bit lower than normal.

Offline Vijay

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Re: nightmare batches!!!
« Reply #20 on: August 04, 2022, 01:10:07 PM »
As Dave says I did mean 1g/l in a liter of meth once the glyc was in and washing. I've only had to do this on a few batches some years ago when I had some real crappy oil that titrated around 7 with sodium. Any soapproduced would have come out with the glyc and they processed well afterwards, thought the final volume was a bit lower than normal.

Sorry guys but I'm confused with the numbers.  So 1g sodium for every litre of oil (so 85g of sodium) mixed with 1l of methanol. Once the glyc is in and washing, pour the methoxide in?  How long should it be mixed for?

Offline countrypaul

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Re: nightmare batches!!!
« Reply #21 on: August 04, 2022, 02:24:45 PM »
I think we have 2 different approachs here.

For the Dr Pepper, if adding the 12g NaOH /50ml Methanol, I would  try half a litre of glyc. If you have some KOH that would require 16g, but if only 90% then 18g. I was following Dave's coment "Suggestion, add the correct chemicals to nuetralise the oil (use a minimum of methanol) to the glycerol you are going to use for the wash. That should leave the oil dry and neutral. I think you would be better off using potassium for the whole method, using sodium for oil that titrates so high is bound to cause issues."

I think Richard is refering to what he used for a batch of his oil previously. We know yours titrates at 12, so just using 1g/L means you would have to repeat the process 12 times. My guess is that Richards glyc also had a significant caustic content, and his oil only titrated at 7.

Offline Vijay

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Re: nightmare batches!!!
« Reply #22 on: August 04, 2022, 03:58:14 PM »
Doing 12g sodium to 50ml meth and 17g pot to 50ml meth at the moment. Not easy mixing that amount of chemicals to the meth though................

Offline countrypaul

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Re: nightmare batches!!!
« Reply #23 on: August 04, 2022, 04:16:17 PM »
Doing 12g sodium to 50ml meth and 17g pot to 50ml meth at the moment. Not easy mixing that amount of chemicals to the meth though................

Difficult, and the possibility of over cooking, which is why I suggested 3-4g at a time... so make sure you do it safely

Offline Vijay

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Re: nightmare batches!!!
« Reply #24 on: August 04, 2022, 04:18:41 PM »
Doing 12g sodium to 50ml meth and 17g pot to 50ml meth at the moment. Not easy mixing that amount of chemicals to the meth though................

Difficult, and the possibility of over cooking, which is why I suggested 3-4g at a time... so make sure you do it safely

I thought you meant add 3-4g of sodium at a time to the 50ml of meth which is what I've done (or trying to lol)

Offline countrypaul

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Re: nightmare batches!!!
« Reply #25 on: August 04, 2022, 04:19:48 PM »
Doing 12g sodium to 50ml meth and 17g pot to 50ml meth at the moment. Not easy mixing that amount of chemicals to the meth though................

Difficult, and the possibility of over cooking, which is why I suggested 3-4g at a time... so make sure you do it safely

I thought you meant add 3-4g of sodium at a time to the 50ml of meth which is what I've done (or trying to lol)

Yes I did.  What did you think I meant out of curiosity?
« Last Edit: August 04, 2022, 04:21:21 PM by countrypaul »

Offline Vijay

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Re: nightmare batches!!!
« Reply #26 on: August 04, 2022, 04:23:46 PM »
when you asked again I wondered if you meant say 4g of meth into 50ml meth x 3 times. I've done it once (so 12g into 50ml)

Offline countrypaul

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Re: nightmare batches!!!
« Reply #27 on: August 04, 2022, 04:33:22 PM »
when you asked again I wondered if you meant say 4g of meth into 50ml meth x 3 times. I've done it once (so 12g into 50ml)

Ah, yes I can see that it could be interpreted that way, but I did mean 12g into 50ml.

Has it all dissolved yet?

Offline Vijay

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Re: nightmare batches!!!
« Reply #28 on: August 04, 2022, 04:36:15 PM »
potassium did and sodium mostly lol

Offline Vijay

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Re: nightmare batches!!!
« Reply #29 on: August 04, 2022, 05:20:15 PM »
Got very dark oil - thought there was no glycerol drop but using a torch behind the sample bottles, I can see the glyc dropped. I'll leave it overnight and titrate both samples in the morning.

I could be wrong, but it looks like the potassium sample oil is slightly lighter than the sodium one