Author Topic: nightmare batches!!!  (Read 13507 times)

Offline countrypaul

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Re: nightmare batches!!!
« Reply #30 on: August 04, 2022, 07:06:34 PM »
What stage are you at? Have you removed the glyc from the enhanced prewash and processed, or is it the glyc of the prewash you are lokking at?

Offline Vijay

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Re: nightmare batches!!!
« Reply #31 on: August 04, 2022, 07:12:49 PM »
Only at the glyc prewash stage (the 12g and 50ml stuff to 1l of oil). Will let that settle overnight and then do a titration

Offline countrypaul

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Re: nightmare batches!!!
« Reply #32 on: August 04, 2022, 10:52:05 PM »
Good luck.

I won't be around until late afternoon tomorrow.

Offline Vijay

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Re: nightmare batches!!!
« Reply #33 on: August 05, 2022, 09:09:27 AM »
I'm totally impressed guys. Sodium is now titrating at 6 and potassium at 4 - can't believe it worked soooo well :)

So should I upscale and go with potassium - for 85l =1445g potassium and 4.25l meth?

Gonna be a lot of chemicals in all by the time I process though isn't it..................

Or do I just process it as normal with 1445g of POTASSIUM and 18l meth?

Just did a test sample of 17g pot and 220ml meth and I'm pretty sure I have glyc drop - but the top bio layer is very dark. I can only tell the drop out by using a torch behind the bottle. Can bio be dark as I've never had that before?

Also there seems to be no soap made with the potassium sample where there was loads with the sodium sample
« Last Edit: August 05, 2022, 12:58:36 PM by Vijay »

Offline countrypaul

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Re: nightmare batches!!!
« Reply #34 on: August 05, 2022, 03:35:01 PM »
One disavantage of potassium soap is that it can take a long time to drop out compared to sodium, as a result often a mixture is used part NaOH and part KOH to get the benefits of both.

As your oil is still titrating quite high (6 or 4), I would be tempted to try with a little more NaOH/KOH and see if you can get that titration level down further, maybe only 5g of NaOH, or 3g KOH (if you have the samples left). The reason being that when you add alot of caustic (soda or potash) there will be  a certain amout of neutralisation, but also an amount of direct saponification where the oil is turned directly to soap. The presence of the glycerol should help reduce this, but given the titration values you now quote it does appear that is happening.

If you remove the glyc, the oil will still contain some soap so trying to transesterify immediatey is likely to produce yet more soap and also give a very incomplete reaction. The problem with an incomplete reaction is that it can result in soap/methanol remaining in the oil/bio and maybe not dropping out at all. More likely to happen with KOH as that tends to take longer anyway.

Due to the high amount of caustic used wit the oil, it is quite likely to go dark, most should drop out with the glyc, but the presence of pattially reacted oil in the form of mono and di glycerides will tend to keep lots of things from dropping. As you get closer to a pass, you should find the glyc drops quicker and the bio gets lighter. The final bio is still likely to be darker that you are used to though.

PS.

I went upto Father's on Teeside as planned and only been there 20 mins before getting a phone that our 10yo had collapsed and an ambulance called - he is home and seems to be none the worse - but I obviously had a change of plan and returned early.


Offline Vijay

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Re: nightmare batches!!!
« Reply #35 on: August 05, 2022, 03:42:10 PM »
Is your ten year old ok, what happened bud??

Offline Vijay

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Re: nightmare batches!!!
« Reply #36 on: August 05, 2022, 04:11:41 PM »
Should have been clearer in my earlier post, when I said "Just did a test sample of 17g pot and 220ml meth and I'm pretty sure I have glyc drop - but the top bio layer is very dark. I can only tell the drop out by using a torch behind the bottle. Can bio be dark as I've never had that before?"         I should have said that is with the oil in my processor, NOT one of the earlier samples with the glyc wash.

I've also done a 3/27 test on that bio and it has stayed cloudy but absolutely no dropout. So a pass yes?

So what would happen if I tried to process it with 1445g pot and 18l of meth?  I do demeth using a condenser which I believe will help let soaps drop when I settle?
« Last Edit: August 05, 2022, 04:36:23 PM by Vijay »

Offline countrypaul

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Re: nightmare batches!!!
« Reply #37 on: August 05, 2022, 05:28:13 PM »
10yo seems fine, he spent quite some time in the swiming pool and had problems when he got out, the ambulance medics think he got too hot in the pool and lost blood pressure when he got out. An hour after he collapsed he was chatting to everyone and appeared fine, and when I got home he was back to normal - Dad can ou fix...

A cloudy 3/27 test can be due to mono and di glycerides being present so I would not class it as a pass. Continue processing for a while longer, or drop teh glyc and reprocess with a small amount of reagents.

Offline Vijay

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Re: nightmare batches!!!
« Reply #38 on: August 05, 2022, 05:52:04 PM »
really glad he's fine, what a worry to get that sort of phone call...................

Offline Vijay

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Re: nightmare batches!!!
« Reply #39 on: August 05, 2022, 05:54:29 PM »
10yo seems fine, he spent quite some time in the swiming pool and had problems when he got out, the ambulance medics think he got too hot in the pool and lost blood pressure when he got out. An hour after he collapsed he was chatting to everyone and appeared fine, and when I got home he was back to normal - Dad can ou fix...

A cloudy 3/27 test can be due to mono and di glycerides being present so I would not class it as a pass. Continue processing for a while longer, or drop teh glyc and reprocess with a small amount of reagents.

This was only a 1l sample but I'm tempted to process the whole lot in one go with all the chemicals on Monday and see how it comes out................

Offline dgs

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Re: nightmare batches!!!
« Reply #40 on: August 05, 2022, 09:52:46 PM »
Been following Paul, pleased your little one is ok.
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline countrypaul

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Re: nightmare batches!!!
« Reply #41 on: August 06, 2022, 08:17:11 AM »
Thanks Vijay and Dave, he is fine now, doesn't like getting up in the morning so he seems back to his usual self

Offline Vijay

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Re: nightmare batches!!!
« Reply #42 on: August 08, 2022, 04:31:58 PM »
so glad to hear that Paul  :)

Well the batch didn't work, didn't get any glyc dropping in hours - not sure whether to laugh or cry right now lol

Offline Vijay

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Re: nightmare batches!!!
« Reply #43 on: August 09, 2022, 09:45:56 AM »
gonna try some sample tests I guess, maybe 2g potassium with 50ml meth?

Well no glyc droped, so up the potassium or meth or both?

Tried 5g pot and 50ml meth and got a small amount of bio on top (like maybe 5%). Any idea which ingredient to change?
« Last Edit: August 09, 2022, 02:53:53 PM by Vijay »

Offline countrypaul

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Re: nightmare batches!!!
« Reply #44 on: August 09, 2022, 03:32:19 PM »
Titrate the "oil" and see what figure you get. If the oil is already akaline then I would assume enough caustic is present and add just methanol - probably another 50m.l If it comes out as still acidic then treat as fresh oil with that titration figure. There may be an area in the middle where it is caustic but not enough to react - in this case I would add 50mlf methanol with 5g of KOH.

Potassium is well known for taking longer to settle out you may have to leave it a few days (though the warm weather may help).

If you have lots of soap it may also take longer for the glyc to drop - one possible approach is to add more glyc to see if that triggers better separation.

Others may give you better directions as I have not used KOH for bio.