Water washing and titrated soap tests.

[Tony]

Very interesting results Nige.

I'm thinking this information should be on the water washing page in some form to give an idea of what to expect when following this method.

[Head Womble]

Very god results there Nige, a testament to your methods.

[nigelb]

Very good results there Nige, a testament to your methods.

When you keep it simple the results are favourable.

A lesson to be learnt here for some...don't over complicate your process.

Nige

[Bill]

Don't know if I've missed something but when you'all have been testing at successive water washes for soap has the bio been wet with water(orange juice) or dried(clear) before measuring out for the soap test.
Thinking about replicating the test with my multiple water wash arragement. Just want to compare like with like test method.

[Soft top]

I tested the wet orange juice.

[nigelb]

Bill...all testing on my part was done with bio straight from the wash tank. In answer to your question...orange juice.

I think the danger of testing with a dried/demethed  sample would be that any soaps present may well drop to the bottom of whatever you have the sample in and could effect the results.

Nige

[Head Womble]

After seeing Nige's results I thought I'd do some tests of my own.

I started with 200L of condenser dried and gly washed oil,
add 3.5L of ASM and 24.5L of meths for the first stage,
0.5ml dropout in the 10/90,
200ml of ASM and 4L of meths add for the second stage,
30min later crystal clear 10/90

I only got 20L of gly out on the first stage (normally 30 to 35 with NaOH),
as I wanted to do a 5% water prewash I added a few liters of gly from the first stage back in so not to form an emulsion.

I took samples at each stage for soap testing.

Raw bio, 1.2ml used (0.61 x 10 = 6.1) 6.1 x 304 = 1854.4ppm, quite surprised at this as I thought it was low compared with Nige's results, so I tested it three times and used the highest result.

5% Prewashed bio 1.77 x 304 = 538ppm

1st wash 0.62 x 304 = 188.48ppm

2nd wash 0.22 x 304 = 66.88ppm

3rd wash 0.04 x 304 = 12.16ppm

All stages were pump washed with 20L of water.

So including the prewash I've used just 70L of water on 200L of bio.

[1958steveflying]

After seeing Nige's results I thought I'd do some tests of my own.

I started with 200L of condenser dried and gly washed oil,
add 3.5L of ASM and 24.5L of meths for the first stage,
0.5ml dropout in the 10/90,
200ml of ASM and 4L of meths add for the second stage,
30min later crystal clear 10/90

I only got 20L of gly out on the first stage (normally 30 to 35 with NaOH),
as I wanted to do a 5% water prewash I added a few liters of gly from the first stage back in so not to form an emulsion.

I took samples at each stage for soap testing.

Raw bio, 1.2ml used (0.61 x 10 = 6.1) 6.1 x 304 = 1854.4ppm, quite surprised at this as I thought it was low compared with Nige's results, so I tested it three times and used the highest result.

5% Prewashed bio 1.77 x 304 = 538ppm

1st wash 0.62 x 304 = 188.48ppm

2nd wash 0.22 x 304 = 66.88ppm

3rd wash 0.04 x 304 = 12.16ppm

All stages were pump washed with 20L of water.

So including the prewash I've used just 70L of water on 200L of bio.

And no emulsions at all with pump washing. very good mate. no acid too.. even better.

[Head Womble]

Hifly (Vince) was the first to do it, or go public with it anyway.
Read this thread
http://www.vegetableoildiesel.co.uk/forum/viewthread.php?tid=26828
So I thought I'd give it a try as ASM is supposed to produce far less soap to start with.
Overall I'm very pleased with the outcome.

[nigelb]

Congratulations Mark. A great set of results.

I suppose I am also quite relieved as it backs up what I've done for years. This should keep any "Doubting Thomas's" quiet. As Steve says...no acid! And no acetone!

What do you plan next Mark...doing the same tests with a bit of acetone? Or stick with this method for a few batches?

Interesting.....the ppm value of the raw bio! I'm looking forward to doing that test again when I next batch up.

How long did it take from start to finish with the washes (as a complete process) and what were your settling times when the pump was turned off?

[Head Womble]

I plan to do a few more batches like this t hopefully prove it's not a one off.

The raw bio result was supprising,
I tested it three times a double checked the calculations as I was sure I'd got the decimal point in the wrong place to start with.
Just to make sure could you check them for me,
1.2ml of bio was used (10% of the normal volume),
lowest amount of 0.01 acid solution used was 0.55ml (1672ppm), highest was 0.61ml (1854.4ppm).

As far as using the acetone goes, seeing Julians results of doing further washes after the acetone wash spurred me on to try this myself,
I had the same result as Julian, so I'm now wondering if the acetone holds the soaps in suspension for a 50/50 test,
but as the titrated soap tests were done after an acid wash (the acid wash interfears with the soap tests) these looked good as well. 
This is why I've removed the acetone washing page from the wiki, at least until more tests can be done.

My daughter has hidden her acetone as she said I was using to much of it, so I can't backup my theory on this as yet.

I did the batch on Thursday, gly washing in the morning then reacting later in the day, then prewashing and settling over night, dog walking and other stuff was done as well so I couldn't devote the hole day to bio.
Friday I did the three washes and dried it (with condenser) and bubbled off the remaining water overnight.
Each wash was pumped for 30 min and settled for at least 2hrs.

[nigelb]

What sort of pump are you using and what's it's flow rate? Was the pump going full tilt throughout the washes? I'm asking because I may have a go at pump washing.

[nigelb]

I plan to do a few more batches like this t hopefully prove it's not a one off.

Good man..that's the way forward with any sort of experimentation and testing

[Head Womble]

What sort of pump are you using and what's it's flow rate? Was the pump going full tilt throughout the washes? I'm asking because I may have a go at pump washing.

I have a 110plm centrifugal pump, and run the eductor during all the wash stages.
The eductor gives me over 500plm of mixing, that's 2 1/2 x batch volume per minuet (educator dimensions and flow calculations from our Jim).

So all washing was quite vigorous, looking back I was lucky to get away without an emulsion on the first wash,
it does prove the method quite well with this in mind.

First wash was at about 45°C.