Author Topic: The no titration two stage process.  (Read 4854 times)

Offline DavidA

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Re: The no titration two stage process.
« Reply #15 on: December 01, 2021, 11:42:49 PM »
I mixed up 30 ml Meth with about 3G NaOH and added it to the original. I see what happened tomorrow.

I did think at the time that hardly any reaction appears to have taken place.

Offline nigelb

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Re: The no titration two stage process.
« Reply #16 on: December 02, 2021, 09:40:43 AM »

I must admit IMO those wiki instructions are to say the least not very good. That 80/20 split of the 2 stages just isn't accurate enough if you water wash. No wonder people end up with emulsions!
Why dont you re-write it Dave. Nothing wrong with an update.
I dare say that some emulsions are caused by bad practice rather than bad reactions.

Offline Keef

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Re: The no titration two stage process.
« Reply #17 on: December 02, 2021, 10:28:23 AM »

I must admit IMO those wiki instructions are to say the least not very good. That 80/20 split of the 2 stages just isn't accurate enough if you water wash. No wonder people end up with emulsions!
Why dont you re-write it Dave. Nothing wrong with an update.
I dare say that some emulsions are caused by bad practice rather than bad reactions.
Sadly, I think It's been some years since we were able to edit or create on the Wiki.  I don't know exactly what the problem is but we are unable to log in anymore  :(

Offline DavidA

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Re: The no titration two stage process.
« Reply #18 on: December 02, 2021, 12:30:21 PM »
I mixed up 30 ml Meth with about 3G NaOH and added it to the original. I see what happened tomorrow.

I did think at the time that hardly any reaction appears to have taken place.

A quick look this morning shows quite a lot of drop-out.

I'll check it properly when things have warmed up a bit. It's only about +5C in the shed at the moment.

Offline dgs

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Re: The no titration two stage process.
« Reply #19 on: December 02, 2021, 01:46:33 PM »
You can actually calculate the rough titration from the dropout.
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline nigelb

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Re: The no titration two stage process.
« Reply #20 on: December 02, 2021, 03:51:48 PM »

Sadly, I think It's been some years since we were able to edit or create on the Wiki.  I don't know exactly what the problem is but we are unable to log in anymore  :(

That's incorrect Keef. I've just logged into the wiki and put in a small edit on the ASM page.??

Offline DavidA

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Re: The no titration two stage process.
« Reply #21 on: December 02, 2021, 04:27:56 PM »
I mixed up 30 ml Meth with about 3G NaOH and added it to the original. I see what happened tomorrow.

I did think at the time that hardly any reaction appears to have taken place.

A quick look this morning shows quite a lot of drop-out.

I'll check it properly when things have warmed up a bit. It's only about +5C in the shed at the moment.


Has a close look  this sample .
It  has 1Litre of clear bio above 0.3 Litre of byproducts.  At 8.2C

A 3/27 test shows no visible drop out. (I'll do another one later).

Update.

Did another drop-out test.

No visible drop out after four hours.
« Last Edit: December 02, 2021, 05:38:35 PM by DavidA »

Offline dgs

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Re: The no titration two stage process.
« Reply #22 on: December 02, 2021, 05:56:18 PM »
I mixed up 30 ml Meth with about 3G NaOH and added it to the original. I see what happened tomorrow.

I did think at the time that hardly any reaction appears to have taken place.

A quick look this morning shows quite a lot of drop-out.

I'll check it properly when things have warmed up a bit. It's only about +5C in the shed at the moment.


Has a close look  this sample .
It  has 1Litre of clear bio above 0.3 Litre of byproducts.  At 8.2C

A 3/27 test shows no visible drop out. (I'll do another one later).

Update.

Did another drop-out test.

No visible drop out after four hours.

So are you saying that you have complete conversion after adding 3.5 + 3.0 gms of NaOH. Did you discard the glycerol after the 1st stage.

Why are you still doing a 3/27 when you now have the proper 10/90 tube.
« Last Edit: December 02, 2021, 05:57:55 PM by dgs »
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline DavidA

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Re: The no titration two stage process.
« Reply #23 on: December 02, 2021, 07:01:07 PM »
I mixed up 30 ml Meth with about 3G NaOH and added it to the original. I see what happened tomorrow.

I did think at the time that hardly any reaction appears to have taken place.

A quick look this morning shows quite a lot of drop-out.

I'll check it properly when things have warmed up a bit. It's only about +5C in the shed at the moment.


Has a close look  this sample .
It  has 1Litre of clear bio above 0.3 Litre of byproducts.  At 8.2C

A 3/27 test shows no visible drop out. (I'll do another one later).

Update.

Did another drop-out test.

No visible drop out after four hours.

So are you saying that you have complete conversion after adding 3.5 + 3.0 gms of NaOH. Did you discard the glycerol after the 1st stage.

Why are you still doing a 3/27 when you now have the proper 10/90 tube.

No. Because I got such a low drop-out with the first part (no drop out) I decided to write off this test.
I added the extra 3g and the bit of methanol to the whole batch, brought it back up to 50C , shook it vigorously and let it settle out as one would for a normal mixing.That way I should at least get some useable fuel from it.
My reasoning was that I may as well do what was essentially a normal mix with 6.5 g of NaOH and see if it worked. I used the 3/27 test as it was the one I normally used in earlier tests. The 10/90 tube can be used in future tests as it is indeed easier to read.

I am going to try the two stage method with 5g for the first stage.

Offline Keef

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Re: The no titration two stage process.
« Reply #24 on: December 02, 2021, 10:22:36 PM »

Sadly, I think It's been some years since we were able to edit or create on the Wiki.  I don't know exactly what the problem is but we are unable to log in anymore  :(

That's incorrect Keef. I've just logged into the wiki and put in a small edit on the ASM page.??
How long has that been possible, no one tells me nothing!!!!

Offline nigelb

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Re: The no titration two stage process.
« Reply #25 on: December 02, 2021, 11:04:05 PM »
Even though I was logged in on the forum I had to log in seperately on the wiki. I then did a small edit regarding the availability of ASM.

Offline dgs

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Re: The no titration two stage process.
« Reply #26 on: December 04, 2021, 08:57:56 PM »
DavidA, it may be helpful to you to go through my process for making bio in cubies. I know you want to make really good bio but its really hard to water wash using this method, best to bubble/settle then woodchip, you will still get to zero soap.

When you have processed to your liking (clear 10/90 of whatever) leave to stand overnight.

Pour the bio into another container, try to make sure you pour as little glyc in as possible.

Bubble for 24 hours

Leave to stand for 24 hours.

Pour through oak woodchips (make sure you pour NO glycerol into the chips) You can then use the bio. If you check for soap it should be zero.

You can gather all the residual glyc with a small amount of bio and use it to glyc wash some more oil, you can do this in a cubie as well. Everything can be done at ambient, I've made bio in cubies outside at about +5degs.
FOC water tests by Sandy brae or Karl Fischer for forum members.

Offline DavidA

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Re: The no titration two stage process.
« Reply #27 on: December 05, 2021, 04:55:33 PM »
Dave (dgs),

I do agree with you regarding the water wash. That is why I never bothered in the past.

I am sending off for a fish tank air pump and will concentrate on bubble washing in the future.

While I am concerned  for the environment, I am no hard-line greenie. Everything is related to cost. And as I am on a water meter, a 40 Watt air pump seems the way to go. Possibly cheaper to run than a water pump.

I did all my past mixing in 20 Ltr poly drums and found them quite usable. I avoided the cubies as they, or at least the ones I got, were attacked by rats who nibbled through them wasting all the oil. They don't seem interested in the poly drums.

Just need to find out where to get oak chips from. Do they have to be oak ?

More tests with things like 80/20 method still to do. I think I will use 5g/Ltr of oil rather than the 3g  (was it 3 or 3.5 ?)  for the 80% bit. May get some dropout that way.

Offline nigelb

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Re: The no titration two stage process.
« Reply #28 on: December 05, 2021, 10:41:23 PM »
I made a batch of 160lt on Saturday and used a base of 6gm/lt for stage one. It gave me a 20% under reaction. Just where I thought it would be. Next batch will be 7gm. I'm now getting my oil from one source. That should see somewhere close to 10% undercook.

3.5gm should be ok for brand new SVO. If the oil has been used there will be FFA in there which will need to be neutralised....hence the increase in catalyst.
« Last Edit: December 05, 2021, 10:44:55 PM by nigelb »

Offline dgs

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Re: The no titration two stage process.
« Reply #29 on: December 05, 2021, 11:08:16 PM »
I made a batch of 160lt on Saturday and used a base of 6gm/lt for stage one. It gave me a 20% under reaction. Just where I thought it would be. Next batch will be 7gm. I'm now getting my oil from one source. That should see somewhere close to 10% undercook.

3.5gm should be ok for brand new SVO. If the oil has been used there will be FFA in there which will need to be neutralised....hence the increase in catalyst.

I don't usually process any oil that titrates. It comes out of my glyc wash ibc. As its glyc washed about 5 times it shows a conversion of about 20% so I'm on 6.5gms K + 10% methanol.
FOC water tests by Sandy brae or Karl Fischer for forum members.