Author Topic: In processor titrated water wash method  (Read 109604 times)

Offline Julian

  • Administrator
  • Oil baron
  • *******
  • Posts: 6389
    • Used Cooking Oil Collection website
  • Location: East Surrey, UK.
Re: In processor titrated water wash method
« Reply #15 on: October 01, 2012, 07:05:13 PM »
And who appointed you as official OTT ... Off Topic Tosser?

I thought I was doing rather well with my Skype thread, that ran to 5 pages mainly on Discos.  I've got lots more to report, but it makes me look a bit of a Muppet, so I may not bother!

Oh, and maybe the info archive is not such a bad idea.
Used Cooking Oil Collection website ... http://www.surreyusedcookingoilcollection.palmergroup.co.uk

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #16 on: October 01, 2012, 08:56:39 PM »
Where has Jules got to?,my process was basically following his first attempt but with a different acid,it wouldnt be fair for me to post it up before his

Offline Julian

  • Administrator
  • Oil baron
  • *******
  • Posts: 6389
    • Used Cooking Oil Collection website
  • Location: East Surrey, UK.
Re: In processor titrated water wash method
« Reply #17 on: October 01, 2012, 09:00:10 PM »
Where has Jules got to?,my process was basically following his first attempt but with a different acid,it wouldnt be fair for me to post it up before his

Oh, seems a shame to waste a thread if Jules isn't going to post ... shall I tell you about my Discovery instaed?
Used Cooking Oil Collection website ... http://www.surreyusedcookingoilcollection.palmergroup.co.uk

Offline julesandtash

  • Wiki Editor
  • Oil obsessive
  • *****
  • Posts: 880
    • Veg oil collection in South East Cornwall
Re: In processor titrated water wash method
« Reply #18 on: October 01, 2012, 09:23:08 PM »
Hi,
I do apologise for not posting, I haven't been on here or VOD for a few days now as it's all been a bit manic here. I have barely had a spare waking moment for various reasons.

Anyway, I am back now.

I can vouch for this method working really well.  I have done three batches in this way now, with different feedstocks and have had perfect results every time.

I do the two stage no titration method with methylate to get a perfect 5/45 test. Then drain the second stage glycerol.

To titrate the bio I made up a titration fluid of 1ml of 96% sulphuric acid in 1 litre of water. The titration itself is carried out with 50ml of IPA with enough drops of Bromophenol blue in it to make it a visible blue colour.
I then drop in 1ml of the bio which, being alkaline, keeps the solution blue
Then, using a 0.5ml syringe, I drip in the 0.1% acid solution and keep stirring until the solution turns greenish yellow.
At that point it is really easy to calculate how much acid is needed.
If the titration took 0.75 ml of acid solution then the bio will need 0.75ml per litre to neutralise.
On a 100 litre batch that would be 75 ml of acid.

Clearly, adding 75ml of concentrated sulphuric acid would carbonise the bio it touched so firstly I mix the acid with the 7% batch volume of water as Paul suggests above.

*** Safety warning - ALWAYS add the acid to the water. NEVER add water to concentrated sulphuric acid as the exothermic reaction will cause the water to instantly boil and throw acid out of the mixing vessel ***

Then mix, stop and allow the water to settle.

The water that comes out is dirty and, with suplhuric acid at least, smelly.
After this, I do another wash with 20% batch volume of clear water. Only needs 10 to 20 mins of mixing then a short time to settle.
The water coming out is then almost crystal clear. I take a sample before switching off the pump so I can see it settle in a jar.

If the water is not crystal clear, I do another wash. So far I have not had to do more than two 20 minute washes to have sparkling clear water coming out.

Then it is just a case of drying, which I also do in the processor with a bubble ring and koi air pump. After that, the bio is ready to use.

Doing one of Nigel's soap tests shows 0 ppm of soap too.

« Last Edit: October 15, 2012, 10:40:35 PM by julesandtash »
7+ years of making bio.
1997 RangeRover P38A 2.5DSE and 2001 Audi Allroad 2.5 V6 Tdi all on B100
Home heating and hot water system on Palm based B100 and Aarrow 7KW wood burner on glycerol logs

Offline Julian

  • Administrator
  • Oil baron
  • *******
  • Posts: 6389
    • Used Cooking Oil Collection website
  • Location: East Surrey, UK.
Re: In processor titrated water wash method
« Reply #19 on: October 01, 2012, 09:32:56 PM »
Sounds good.  Maybe I'll try using some of my Sulphuric after all.

I'm guessing you have a bit of a head start over others with the Methylate.
Used Cooking Oil Collection website ... http://www.surreyusedcookingoilcollection.palmergroup.co.uk

Offline julesandtash

  • Wiki Editor
  • Oil obsessive
  • *****
  • Posts: 880
    • Veg oil collection in South East Cornwall
Re: In processor titrated water wash method
« Reply #20 on: October 01, 2012, 09:43:16 PM »
I think the only thing Methylate brings to the party is potentially less soap in the bio due to the lack of water produced.
NaOH or KOH would work just as well except that slightly more acid may be needed.
Sulphuric acid is so cheap and you need to little that I suspect it may work out cheaper than vinegar.

I have given some acid and Bromophenol blue to Bob (Photoman290 on VOD) for him to have a go with in his new processor.

Using this method really reduces the amount of kit needed.
No need for a separate bubbling/settling tank and no need for a consdenser as there is no methanol to recover (the small amount left in the bio after draining the second stage glyc goes out with the wash water).
If you use pre-pump injection of methoxide then there is no real need for a venturi and, if you get the oil to full process temperature before it goes into the processor (using a boiler, electric overnight heating etc) then you dont even need and inline or in processor heater.

I get my oil to 70C at the start of the day. Then glyc wash, then two stage process then in processor water was by this method.
Even after two cold water washes the bio is still at 35C to 40C at the end of  the process with no extra heat added at any stage.
7+ years of making bio.
1997 RangeRover P38A 2.5DSE and 2001 Audi Allroad 2.5 V6 Tdi all on B100
Home heating and hot water system on Palm based B100 and Aarrow 7KW wood burner on glycerol logs

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #21 on: October 01, 2012, 09:44:26 PM »
Im still on NaOH but it seems to work well,i wont say just as well as i haven't tested the soap PPM but i have got crystal clear water in the 50/50,i have got some acids here but thought i would try vinegar to differ from Jules,the processor seems already set up for this and now the wash tank will just be a drying tank,i suppose some will never get over the fear of adding water but i consider this a step forward
I await the "its been tried 5 years ago" with interest

Offline Keef

  • Administrator
  • Oil obsessive
  • *****
  • Posts: 552
    • Adur Cooking Oils
  • Location: Sussex
Re: In processor titrated water wash method
« Reply #22 on: October 01, 2012, 09:44:47 PM »
Has anyone tried titrating the finished bio?

If the acid turns the soaps to FFAs, are you sure they are all washed out during the washes or have you got acid bio?

Just a thought.

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #23 on: October 01, 2012, 09:45:31 PM »
I think the only thing Methylate brings to the party is potentially less soap in the bio due to the lack of water produced.
NaOH or KOH would work just as well except that slightly more acid may be needed.
Sulphuric acid is so cheap and you need to little that I suspect it may work out cheaper than vinegar.

I have given some acid and Bromophenol blue to Bob (Photoman290 on VOD) for him to have a go with in his new processor.

Using this method really reduces the amount of kit needed.
No need for a separate bubbling/settling tank and no need for a consdenser as there is no methanol to recover (the small amount left in the bio after draining the second stage glyc goes out with the wash water).
If you use pre-pump injection of methoxide then there is no real need for a venturi and, if you get the oil to full process temperature before it goes into the processor (using a boiler, electric overnight heating etc) then you dont even need and inline or in processor heater.

I get my oil to 70C at the start of the day. Then glyc wash, then two stage process then in processor water was by this method.
Even after two cold water washes the bio is still at 35C to 40C at the end of  the process with no extra heat added at any stage.

Stone the blasphemer!

sorry couldnt resist

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #24 on: October 01, 2012, 09:46:09 PM »
Has anyone tried titrating the finished bio?

If the acid turns the soaps to FFAs, are you sure they are all washed out during the washes or have you got acid bio?

Just a thought.
Mine tested at 7.5

Offline julesandtash

  • Wiki Editor
  • Oil obsessive
  • *****
  • Posts: 880
    • Veg oil collection in South East Cornwall
Re: In processor titrated water wash method
« Reply #25 on: October 01, 2012, 09:49:52 PM »
I take it that was a pH of 7.5 as opposed to a titration value of 7.5 (which would be quite seriously acidic).

7+ years of making bio.
1997 RangeRover P38A 2.5DSE and 2001 Audi Allroad 2.5 V6 Tdi all on B100
Home heating and hot water system on Palm based B100 and Aarrow 7KW wood burner on glycerol logs

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #26 on: October 01, 2012, 09:52:26 PM »
Yes,sorry pH
I found this when hunting down the indicator,may be of some use


Offline Julian

  • Administrator
  • Oil baron
  • *******
  • Posts: 6389
    • Used Cooking Oil Collection website
  • Location: East Surrey, UK.
Re: In processor titrated water wash method
« Reply #27 on: October 01, 2012, 09:53:38 PM »
Can you measure the ph of Bio? I thought you could only measure the ph of water based liquids.
Used Cooking Oil Collection website ... http://www.surreyusedcookingoilcollection.palmergroup.co.uk

Offline K.H

  • Administrator
  • Oil baron
  • *******
  • Posts: 2353
  • Location: Tosser towers
Re: In processor titrated water wash method
« Reply #28 on: October 01, 2012, 09:55:06 PM »
Can you measure the ph of Bio? I thought you could only measure the ph of water based liquids.
Used a couple of indicators to get a rough idea,not very scientific admittedly

Offline mark230678

  • Barrel scraper
  • *
  • Posts: 13
Re: In processor titrated water wash method
« Reply #29 on: October 01, 2012, 09:57:55 PM »
Am watching this with interest, as my processor will be built over the weekend.( Hopefully )
I used to water wash (mist) about 4 the the volume of bio.
This sounds perfect.